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Piperidine

Piperidine is a six-membered saturated with the molecular formula C₅H₁₁N, in which one of the carbon atoms in a ring is replaced by a atom. Also known as hexahydropyridine or azinane, it serves as a secondary and exists as a clear, colorless liquid with a pepper-like odor at room temperature. Piperidine exhibits basic properties due to its atom, with a of 11.12 for its conjugate acid, making it a strong base that reacts exothermically with acids. Its physical properties include a of 106 °C, a of -9 °C, a of 0.862 g/cm³, and high flammability with a of 16 °C; it is miscible with and many solvents. Industrially, piperidine is primarily synthesized by the catalytic hydrogenation of using or catalysts. As a versatile chemical intermediate, piperidine is widely used in the production of pharmaceuticals, rubber accelerators, epoxy curing agents, and as a solvent in organic synthesis. It also finds applications in peptide synthesis for Fmoc group removal and as a structure-directing agent in zeolite preparation. Biologically, piperidine occurs naturally as a metabolite in humans and plants such as Cannabis sativa, and it is classified as a high-production volume chemical in the United States, exceeding 1 million pounds annually. However, it is corrosive to skin and eyes, toxic if inhaled or ingested (with an oral LD50 in rats of 337 mg/kg), and requires careful handling due to its flammability and vapor hazards.

Structure and Properties

Molecular Structure

Piperidine is a saturated with the molecular formula \ce{C5H11N}. It features a six-membered structure comprising five methylene (\ce{CH2}) groups and one secondary amine (\ce{-NH}) group, where the occupies one position in the . This arrangement positions the as a , replacing a carbon in an analogous all-carbon cycle. In comparison to cyclohexane (\ce{C6H12}), which consists entirely of carbon atoms in a six-membered ring, piperidine substitutes one methylene group with an imino (\ce{-NH}) unit. This heteroatom replacement introduces a lone pair of electrons on the nitrogen, altering the electronic distribution without fundamentally changing the ring size or saturation, though it influences bond characteristics. The static molecular framework remains a cyclic structure with single bonds throughout. Structural representations of piperidine include the skeletal formula, depicted as a simple hexagon with one vertex marked as (N) to denote the connectivity, omitting explicit for clarity. In three-dimensional models, the molecule is shown with the integrated into the , highlighting the secondary amine's attachment. The is piperidine, a retained name for this common heterocycle, while the systematic Hantzsch-Widman name is azinane. The N-C lengths in piperidine measure approximately 1.472 , which is shorter than the typical C-C length of 1.54 found in , attributable to the higher of and the partial sp³ hybridization influenced by its electrons. The angle at the , specifically the C-N-C angle, is about 109.8°, approximating the ideal tetrahedral geometry expected for an sp³-hybridized . These parameters underscore the 's role in modulating the ring's structural rigidity compared to analogs.

Physical Properties

Piperidine is a clear, colorless liquid at , exhibiting a characteristic pepper-like odor reminiscent of due to its functionality. Key physical constants of piperidine under standard conditions include a of 106 °C at 760 mm , a of -9 °C, a density of 0.862 g/cm³ at 20 °C, and a of 1.453 at 20 °C.
PropertyValueConditions
Boiling point106 °C760 mm
Melting point-9 °C-
Density0.862 g/cm³20 °C
Refractive index1.45320 °C (D line)
Piperidine is miscible with , , and , reflecting its polar nature, and possesses a (log P) of 0.84, indicating moderate suitable for partitioning between aqueous and organic phases. Thermodynamic properties include an of approximately 36.6 kJ/ at 338 , decreasing to 35.3 kJ/ at 357 near its , and a liquid heat capacity of 180 J/· at 298 . The follows the , log10(P) = 3.98189 - (1239.577 / (T - 67.622)), where P is in bar and T in , valid over 315–417 , yielding values such as 32.1 mm at 25 °C and 40 mm at 29.2 °C.

Chemical Properties

Piperidine exhibits strong basicity characteristic of aliphatic secondary amines, with the of its conjugate acid (piperidinium ion) measured at 11.12 in at 25°C. This value indicates moderate basic strength, enabling piperidine to readily accept a proton. Compared to , which has a conjugate acid of 5.17, piperidine is approximately 10^6 times more basic; this difference arises because the in piperidine is sp³-hybridized, positioning its in an orbital orthogonal to the ring and fully available for , whereas pyridine's sp²-hybridized has its in the ring plane, delocalized within the aromatic π-system and less accessible. The N-H proton in piperidine displays weak acidity, with an estimated of approximately 38, reflecting the low tendency of the neutral to lose this proton and form the amidate anion. Due to its fully saturated six-membered ring, piperidine lacks the structural features for tautomerism, such as adjacent carbonyls or unsaturation that could enable keto-enol or imine- shifts. The molecule possesses a of 1.2 D, primarily attributable to the polarity of the nitrogen and the asymmetric charge distribution across the ring. Piperidine demonstrates good stability under neutral conditions but shows sensitivity to strong acids, with which it reacts exothermically to form stable salts. It is also hygroscopic, readily absorbing moisture from the air owing to its and miscibility with . While generally resistant to mild oxidation in ambient environments, piperidine reacts violently with strong oxidizing agents, potentially leading to decomposition or hazardous gas evolution.

Synthesis and Production

Industrial Production

Piperidine is primarily produced on an industrial scale through the catalytic of , which is the most economical and widely adopted method. This process involves reacting with gas in the presence of or catalysts at temperatures ranging from 150 to 200°C and pressures of 10 to 20 atm, yielding piperidine with high selectivity. Commercial piperidine is purified via to achieve purity levels greater than 99% for standard grades, ensuring suitability for industrial applications. Byproducts such as piperideine, an intermediate formed during partial , are managed through optimized reaction conditions and to minimize waste and improve yield. Recent advancements include sustainable routes from biomass-derived feedstocks, such as the catalytic conversion of δ-valerolactone to piperidine, offering potential alternatives to traditional methods as of 2025.

Laboratory Synthesis

One established laboratory method for synthesizing piperidine involves the of with , followed by cyclization. In this approach, reacts with to form an intermediate , which is then reduced using a hydride reagent such as or catalytic , leading to ring closure and piperidine formation. This method is particularly suited for small-scale preparations due to the availability of and its mild conditions, avoiding harsh reagents often required in industrial processes. A variant of the provides another route, utilizing and 1,5-dibromopentane to construct the piperidine ring. undergoes sequential with the dihalide, forming a cyclic N-phthaloyl intermediate that is subsequently deprotected via hydrazinolysis or to afford piperidine. This method offers good selectivity for primary precursors and is valuable in research for incorporating piperidine into more complex structures, though it requires careful control to minimize polymerization side products. Modern laboratory techniques have expanded options for piperidine synthesis, particularly for chiral analogs. Ring-closing metathesis (RCM) of acyclic ene-carbamates or allylic amines, catalyzed by ruthenium complexes like Grubbs' second-generation catalyst, enables efficient formation of the piperidine core with high stereocontrol, often achieving yields above 80% for substituted variants. Complementing this, enzymatic reductions using imine reductases or carbonyl reductases on piperidone precursors provide access to enantioenriched piperidines, with enantiomeric excesses exceeding 95% in biocatalytic cascades. For isotopically labeled variants, deuterated piperidine is prepared by catalytic reduction of with D₂ gas over or catalysts, incorporating deuterium at specific positions for NMR or metabolic studies.

Natural Occurrence

Sources in Nature

Piperidine occurs naturally in (Piper nigrum), where it is present at concentrations of approximately 5 mg/g, contributing to the characteristic peppery odor alongside the more abundant . This compound is one of the major alkaloids extracted from the plant, though in levels lower than (around 20 mg/g in typical samples). In (Nicotiana species), piperidine is detected in cigarette smoke as a volatile , formed likely through degradation during combustion. It is also a natural constituent in mammalian , excreted at levels of several mg/L under physiological conditions. Piperidine has been isolated from , particularly in ethanol extracts of the plant, contributing to its odor profile. Microbial production of piperidine occurs in soil bacteria such as species, where it arises through pathways involving catabolism, including and cyclization steps that yield piperidine or its immediate precursors like Δ¹-piperideine. These bacteria, common in environments, produce piperidine-type compounds as part of , aiding in interspecies interactions.

Biological Derivatives

Piperidine serves as a core scaffold in numerous naturally occurring alkaloids, particularly within plant families such as Piperaceae and Apiaceae, where it contributes to bioactive compounds with defensive roles against herbivores and pathogens. One prominent example is piperine, a piperidine amide with the molecular formula C₁₇H₁₉NO₃, isolated from black pepper (Piper nigrum), which exhibits insecticidal properties by disrupting insect neural function and deterring feeding. Another key derivative is coniine, a simple 2-propylpiperidine alkaloid found in poison hemlock (Conium maculatum), known for its potent neurotoxicity as a nicotinic acetylcholine receptor agonist, leading to paralysis and respiratory failure in animals and humans. Biosynthetically, many piperidine alkaloids derive from the through to form , which cyclizes to piperideine intermediates before incorporation into the final structures, often involving condensation with units; can serve as an alternative precursor in some pathways. For instance, pelletierine, a 2-(3-oxobutyl)piperidine present in ( granatum) root bark, arises via lysine-derived cadaverine condensing with acetoacetyl-CoA, contributing to the plant's antiparasitic defenses against nematodes. Similarly, sedridine, a 2-(1-hydroxypropyl)piperidine isolated from and related species in the family, follows a lysine-based route with stereoselective reduction steps, aiding in deterrence through its bitter taste and mild . These pathways underscore the alkaloids' role in plant defense, enhancing survival by repelling insects and vertebrates. Evolutionarily, the piperidine scaffold underpins over 100 alkaloids in the family alone, reflecting in tropical lineages where these compounds likely evolved for against specialized herbivores, with evidence of in isolated genera like and . This structural motif's prevalence highlights its biochemical versatility and selective advantage in diverse ecological niches.

Conformation and Spectroscopy

Ring Conformation

Piperidine predominantly adopts a conformation, analogous to , in which substituents can occupy axial or equatorial positions relative to the ring. This puckered structure minimizes angle and torsional strain, with the nitrogen atom exhibiting pyramidal geometry due to its . The chair form allows for dynamic interconversion between conformers where the N-H bond is either axial or equatorial, facilitated by low-energy pathways. The interconversion between these chair conformers occurs primarily through nitrogen inversion, an umbrella-like flipping of the pyramidal nitrogen. The free energy barrier for this process is approximately 6.2 kcal/mol at , measured via dynamic NMR . This barrier is lower than that observed in the five-membered analog , where values around 8 kcal/mol have been reported, attributable to the increased flexibility of the six-membered ring that reduces steric constraints during inversion. The equatorial N-H conformer is thermodynamically favored over the axial one by about 0.6 kcal/mol, as established from vibrational spectroscopic analysis and calorimetric measurements in the gas phase. This preference arises from reduced 1,3-diaxial interactions in the equatorial orientation. calculations confirm this energy difference for the unsubstituted ring. Protonation at the atom, forming the piperidinium cation, preserves the overall conformation but introduces electrostatic effects from the positive charge that slightly flatten the ring geometry and elevate the relative energy of boat forms, increasing their population in computational models of the isolated ion.

NMR Spectroscopy

Piperidine's ^1H NMR spectrum in CDCl_3 typically shows the α-protons (positions 2 and 6) as a triplet at 2.20–2.30 due to with adjacent β-protons, integrating for 4H. The β-protons (positions 3 and 5) appear as a multiplet at 1.5–1.6 , integrating for 4H, while the γ-protons (position 4) overlap in this region as a multiplet around 1.4 , contributing to the overall 6H for the aliphatic CH_2 groups. The NH proton resonates as a broad at approximately 1.4 , which can vary slightly with concentration and temperature due to hydrogen bonding and . In ^13C NMR, also recorded in CDCl_3, the α-carbons (C2 and C6) exhibit a chemical shift of about 46 , the β-carbons (C3 and C5) at 26 , and the γ-carbon (C4) at 24 , reflecting the electron-withdrawing influence of the on the adjacent carbons. These values are characteristic of the saturated heterocyclic ring and aid in structural confirmation. Vicinal proton-proton coupling constants (^3J_{H-H}) in piperidine are approximately 7 Hz, consistent with the conformation where angles average due to rapid ring inversion on the NMR timescale, leading to equivalent axial and equatorial positions and simplified splitting patterns. This dynamic inversion, occurring at rates much faster than the NMR observation frequency at , results in time-averaged signals rather than distinct conformer peaks. Solvent effects are pronounced in NMR spectra of piperidine; in non-polar CDCl_3, the free base form dominates, yielding the shifts noted above, whereas in protic D_2O, partial to the piperidinium occurs due to the high basicity (pK_a ≈ 11.2), deshielding the α-protons to around 3.1–3.3 and eliminating the NH signal through deuterium exchange. Piperidine has historically served as a control sample in NMR for calibrating secondary signals and verifying instrument resolution in spectral libraries.

Chemical Reactions

Basicity and Protonation

Piperidine, as a secondary aliphatic , exhibits basic behavior primarily through at the on the atom, yielding the piperidinium cation (C₅H₁₁NH⁺). This is described by the C₅H₁₀NH + H₂O ⇌ C₅H₁₁NH⁺ + OH⁻, with the piperidinium serving as the conjugate . The pKₐ of the piperidinium in at 25°C is 11.12, reflecting piperidine's moderate basic strength relative to other amines. The base dissociation constant (K_b) for piperidine is 1.3 × 10⁻³, corresponding to a pK_b of approximately 2.89. This makes piperidine a significantly stronger than , which has a K_b of 1.8 × 10⁻⁵, by a factor of about 72. The enhanced basicity arises from the inductive electron-donating effect of the two methylene groups attached to the in the six-membered ring, which increase the electron density on the and stabilize the positive charge in the protonated form. Protonation induces distinct spectroscopic shifts that confirm the structural change at . In () spectroscopy, the neutral piperidine shows a characteristic N-H stretching band near 3300 cm⁻¹. Upon to form the piperidinium , this shifts to a broad, intense absorption envelope typically spanning 3000–2500 cm⁻¹, attributable to the asymmetric and symmetric stretches of the -NH₂⁺ group involved in hydrogen bonding. () spectroscopy reveals minimal changes for piperidine itself due to the absence of a conjugated , though can subtly alter any weak n→σ* transitions near 200 nm in the piperidinium salt. The piperidinium ion readily forms stable salts with acids, enhancing and crystallinity for practical use. The hydrochloride salt (C₅H₁₁NH⁺ Cl⁻) is a , hygroscopic crystalline solid with high exceeding 1500 g/L at 20°C and a of 6–8 in (111 g/L). This salt's properties stem from the ionic nature of the protonated paired with the anion, making it more polar and easier to handle than the volatile .

Nucleophilic Additions and Alkylations

Piperidine, being a secondary , serves as a in reactions with electrophiles, particularly with acylating agents. occurs readily with acid chlorides to produce N-acylpiperidines, which are important intermediates in . A representative example is the reaction of piperidine with in at , in the presence of triethylamine as a , yielding N-acetylpiperidine (1-acetylpiperidine) in moderate yields after purification by . This process involves nucleophilic attack by the nitrogen on the carbonyl carbon of the acid chloride, followed by chloride departure and formation of the bond. Similar acylations with other acid chlorides, such as , proceed analogously to afford N-benzoylpiperidine derivatives. The kinetics of acylation reactions between piperidine and acyl chlorides follow second-order rate laws, depending on the concentrations of both the amine and the electrophile, as determined in benzene solutions at 25°C. For instance, studies on substituted piperidines with acetyl chloride reveal rate constants influenced by steric and electronic effects of substituents on the piperidine ring, with unsubstituted piperidine exhibiting relatively high reactivity due to minimal steric hindrance. These second-order rate constants for typical acyl chlorides range from 10^{-2} to 10^{0} L mol^{-1} s^{-1} in non-polar solvents, highlighting the efficiency of the nucleophilic addition mechanism. Alkylation of piperidine with electrophilic alkyl halides, such as , proceeds via successive nucleophilic substitutions to form first N-methylpiperidine and then, under exhaustive conditions, the N,N,N-trimethylpiperidin-1-ium . This quaternization typically occurs in solvents like acetone or at , with excess driving the reaction to completion. exemplifies , where the attacks the carbon of the , and further eliminates the to yield the stable . for such alkylations are also second-order, with rate constants for and piperidine on the order of 10^{-3} to 10^{-1} L mol^{-1} s^{-1} in polar aprotic solvents, reflecting the nucleophilicity of the . Piperidine also undergoes addition to carbonyl compounds, forming enamines through a mechanism involving carbinolamine intermediate dehydration. With aldehydes, this reaction is facilitated under Dean-Stark conditions to azeotropically remove water, promoting the formation of enamines such as those derived from and piperidine (1-(1-propenyl)piperidine). The process requires reflux in or with a catalytic amount of acid, yielding enamines suitable for subsequent alkylation in Stork enamine synthesis. Second-order rate constants for piperidine addition to carbonyls are typically in the range of 10^{-4} to 10^{-2} L mol^{-1} s^{-1} under conditions, underscoring the role of water removal in shifting equilibrium toward the enamine product.

Nucleophilic Substitutions

Piperidine, a secondary , serves as an effective in SN2 displacement reactions with primary alkyl , leading to the formation of N-alkylpiperidine derivatives. For instance, the reaction of piperidine with in solvent yields N-butylpiperidine in 80% isolated yield after stirring at followed by standard . These reactions proceed via a concerted backside attack, where the nitrogen displaces the leaving group, and are favored under mild conditions to minimize over-alkylation due to the basicity of the product . In aromatic nucleophilic substitutions, piperidine participates in palladium-catalyzed reactions with , enabling the of N-arylpiperidines. A representative example involves the coupling of 2-bromotoluene with piperidine using a catalyst in 2,2,5,5-tetramethyloxolane , affording the corresponding N-(2-methylphenyl)piperidine in 88% yield. This cross-coupling tolerates various electron-donating and withdrawing substituents on the , proceeding through , coordination, and steps. Under basic conditions, particularly with secondary or tertiary alkyl halides, E2 elimination can occur as a side reaction during piperidine , producing an and the piperidinium ion instead of the desired substitution product. For example, when piperidine reacts with a secondary alkyl , the strong abstracts a β-proton, leading to and formation of an with concomitant of piperidine. This competing pathway is more pronounced at elevated temperatures or with hindered substrates, reducing the selectivity for SN2 substitution. In SN2 reactions involving chiral alkyl substrates, piperidine induces inversion of at the stereogenic center due to the backside nucleophilic attack. This stereospecificity has been demonstrated in the displacement of a chiral secondary tosylate by piperidine, resulting in the inverted product with high enantiomeric purity. The retention of optical activity but change in underscores the concerted nature of the mechanism.

Applications and Uses

Industrial Applications

Piperidine plays a key role in the rubber industry as a precursor for accelerators. It is primarily converted into dipiperidinyl or tetrasulfide derivatives through reaction with , which function as ultra-accelerators in sulfur-based curing processes for and synthetic rubbers. These accelerators enhance the efficiency of cross-linking, improving the mechanical properties of rubber products such as tires and conveyor belts. This application accounts for a substantial portion of piperidine's demand, with the derivative enabling faster at lower temperatures compared to traditional systems. In the production of materials, piperidine and its alkyl-substituted analogs serve as effective catalysts for the -hydroxyl . These tertiary amines promote the formation of linkages in flexible and rigid foams, as well as coatings and elastomers, by facilitating nucleophilic attack on the isocyanate groups. The use of piperidine-based catalysts allows for controlled reaction rates and reduced processing times, contributing to energy-efficient manufacturing of insulation foams and automotive components. Piperidine derivatives are employed as corrosion inhibitors in oilfield operations, particularly to protect pipelines and equipment from acidic during well stimulation and production. These s adsorb onto metal surfaces, forming protective films that inhibit both anodic and cathodic reactions in environments typical of acidizing treatments. Effective inhibition is achieved at low concentrations, typically ranging from 0.1% to 1% by weight, making them economical for large-scale applications in the sector. As a chemical intermediate, piperidine is utilized in the synthesis of azo dyes and pigments, where it contributes to the formation of heterocyclic structures that provide vibrant colors and . Its nitrogen-containing ring enhances solubility and reactivity in coupling reactions with diazonium salts.

Pharmaceutical Uses

Piperidine serves as a versatile heterocyclic scaffold in , frequently incorporated into drug candidates to modulate pharmacological properties due to its conformational flexibility and basic atom, which facilitates interactions with biological targets. In the development of antagonists, the basic nitrogen of the piperidine ring plays a key role in enhancing receptor binding affinity through and electrostatic interactions with the receptor's , thereby improving antihistaminic potency for treatments. Substituted piperidine derivatives, such as those structurally related to diphenhydramine, exemplify this utility by providing effective H1 blockade while minimizing sedation in second-generation antihistamines. Piperidine is integral to the structure of potent analgesics, particularly in and its analogs, where the 4-anilidopiperidine core confers high affinity for the μ- receptor, enabling superior analgesic efficacy compared to . Modifications to the piperidine ring in these compounds, such as 3-methyl substitutions, further enhance μ-receptor selectivity and potency, with fentanyl analogs demonstrating values in the nanomolar range for opioid binding. The incorporation of piperidine improves the absorption, distribution, metabolism, and excretion () profile of pharmaceutical compounds, primarily through its contribution to molecular , which enhances and membrane permeability. This property allows piperidine-containing drugs to achieve effective systemic exposure following , as seen in various and derivatives. Structure-activity relationship (SAR) studies on piperidine derivatives, dating back to the , have highlighted the profound influence of N-substitution on potency, with alkyl or aryl groups at the position often increasing receptor and therapeutic . For instance, N-benzyl substitutions in piperidine scaffolds have been shown to optimize cholinesterase inhibition in Alzheimer's treatments like donepezil, while similar modifications in analogs from the mid-20th century onward fine-tuned μ-receptor binding to boost activity without excessive side effects. These investigations underscore how N-substituents modulate and steric hindrance to refine pharmacological profiles.

Toxicity and Safety

Health Effects

Piperidine is acutely toxic upon , with an LD50 of 330–740 /kg in rats. Inhalation exposure leads to respiratory irritation, including , coughing, and labored breathing, while dermal and ocular contact causes severe burns and potential permanent tissue damage. Systemic effects from acute exposure may include , , , , and . Chronic exposure to piperidine has been associated with neurotoxic effects and liver impairment in . Piperidine has not been classified by the International Agency for Research on Cancer (IARC) regarding its carcinogenicity to humans. Under the Globally Harmonized System (GHS), it is classified as Category 3 (oral, dermal, inhalation), Corrosion Category 1B, and Category 2. In mammals, piperidine is rapidly absorbed through the , , and skin, and is metabolized primarily in the liver to hydroxylated derivatives such as 3-hydroxypiperidine and 4-hydroxypiperidine in rats. Piperidine poses moderate to aquatic organisms, with an LC50 of approximately 130 mg/L for fathead minnows (Pimephales promelas) over 96 hours. It is biodegradable but can persist in water bodies, contributing to environmental hazards through low potential (BCF of 3) and disruption of aquatic ecosystems.

Handling Precautions

Piperidine is a flammable liquid with a strong , requiring careful handling to prevent and ignition risks. Workers should use it only in well-ventilated areas or under a to minimize of vapors, which can cause respiratory . Avoid generating aerosols or dust, and do not allow the substance to contact skin, eyes, or clothing. Appropriate (PPE) is essential, including tightly fitting safety goggles or face shields compliant with OSHA 29 CFR 1910.133 or EN 166 standards to protect against splashes. Gloves made of (0.7 mm thickness, breakthrough time >480 minutes for full contact) or (0.4 mm thickness, breakthrough time >120 minutes for splash protection) are recommended, along with flame-retardant, antistatic protective clothing. For respiratory protection, use a NIOSH/MSHA-approved respirator with an organic vapor cartridge (Filter A per DIN 3181) if ventilation is inadequate or limits are exceeded. Safe handling practices include washing hands, face, and exposed thoroughly after use, and immediately changing contaminated while applying preventive . Do not eat, drink, or smoke in areas where piperidine is handled to prevent accidental . Keep away from ignition sources, open flames, hot surfaces, and static discharge, as piperidine has a of 16 °C and autoignition temperature of 320 °C. For storage, maintain piperidine in tightly closed containers in a cool, dry, well-ventilated area inaccessible to unauthorized personnel, classified under flammable liquids (Class 3). In case of spills, evacuate the area, ventilate, and absorb with inert material before cleanup, wearing appropriate PPE. Always follow good industrial hygiene practices and consult material safety data sheets for site-specific procedures.