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Menthone

Menthone is a naturally occurring monoterpenoid with the molecular formula C₁₀H₁₈O, commonly found as a of stereoisomers in essential oils such as peppermint oil from Mentha piperita.<grok:render type="render_inline_citation"> 0 </grok:render> It serves as a key precursor to and is characterized by its minty, herbaceous odor, contributing to the cooling sensation in various applications.<grok:render type="render_inline_citation"> 1 </grok:render> The primary isomer, (-)-menthone, has the IUPAC name (2S,5R)-2-isopropyl-5-methylcyclohexan-1-one and appears as a clear, colorless to pale yellow liquid with a of 207–210 °C and density of 0.893 g/mL at 20 °C.<grok:render type="render_inline_citation"> 1 </grok:render> Menthone is soluble in organic solvents like , , and , but has limited in (approximately 496.7 mg/L at 25 °C).<grok:render type="render_inline_citation"> 1 </grok:render> It is extracted from plants in the genus, including and Mentha longifolia, where it can constitute up to 50.9% of the oil in certain varieties.<grok:render type="render_inline_citation"> 0 </grok:render> In industry, menthone is widely used in perfumery and for its aromatic minty profile, as well as in for food and beverages due to its taste threshold of around 50 ppm.<grok:render type="render_inline_citation"> 1 </grok:render> It also finds application in the of agrochemicals and dyestuffs, leveraging its chemical reactivity as a cyclohexanone derivative.<grok:render type="render_inline_citation"> 1 </grok:render> Additionally, menthone enhances salivary flow and activates the TRPM8 receptor, inducing a cold sensation similar to .<grok:render type="render_inline_citation"> 0 </grok:render> Research highlights menthone's biological activities, including , , and neuroprotective effects, making it a component in medicinal preparations for colds, gastrointestinal issues, and topical remedies.<grok:render type="render_inline_citation"> 0 </grok:render> It exhibits antibacterial, antitumor, and antiviral properties, with studies showing suppression of proinflammatory cytokines like IL-1β and TNF in response to LPS stimulation.<grok:render type="render_inline_citation"> 2 </grok:render> Furthermore, menthone demonstrates , mucolytic, , and anti-infective qualities, and can be biotransformed into neomenthol by certain fungi.<grok:render type="render_inline_citation"> 0 </grok:render>

Natural Occurrence and Biosynthesis

Sources in Essential Oils

Menthone, a monoterpenoid ketone, occurs naturally as a key component in the essential oils of various species, particularly those in the family. It is prominently featured in ( × piperita), where it serves as a significant constituent alongside , often comprising 20-30% of the total oil composition in mature plants. In these oils, l-menthone represents the dominant stereoisomer, contributing to the characteristic profile of monoterpenoids derived from . Corn mint (Mentha arvensis), another major source, contains menthone at lower levels, typically 5-10% of the , with l-menthone again predominating as the primary isomer. Pennyroyal () also harbors menthone, though in smaller proportions around 5-7%, where it coexists with pulegone as a notable monoterpenoid. Beyond species, menthone appears as a minor component in the essential oils of geraniums (), reaching up to 6% in some varieties. Concentrations of menthone in these essential oils exhibit regional variations, with higher levels often observed in plants from temperate climates, such as those in Mediterranean or northern European regions, due to environmental influences on accumulation. Within oils, menthone functions as an in the biosynthetic pathway toward production, influencing the overall yield and quality in temperate-growing cultivars. Menthone was first identified as a natural component in essential oils in 1891, initially isolated from .

Biosynthetic Pathways

Menthone is biosynthesized in the glandular trichomes of species primarily through the methylerythritol phosphate () pathway, starting from (GPP), which undergoes sequential enzymatic transformations leading to the formation of the p-menthane skeleton. The process begins with the cyclization of GPP to (-)- catalyzed by (-)-limonene (LimS), followed by to (-)-trans-isopiperitenol by limonene-3-hydroxylase (L3H). Subsequent oxidation by (-)-trans-isopiperitenol (IPDH) yields (-)-isopiperitenone, which is reduced by (-)-isopiperitenone reductase (IPR) to cis- and trans-isopulegone. Isopulegone isomerase (IPGI) then converts these to (+)-pulegone, a key intermediate. From pulegone, the pathway branches: direct stereoselective reduction by pulegone reductase () produces (-)-menthone, while an alternative route involves cyclization to (+)-menthofuran via menthofuran (MFS), a dead-end that can inhibit activity and divert flux away from menthone. The core biosynthetic route to menthone can be represented textually as follows: GPP → (-)- → (-)-trans-isopiperitenol → (-)-isopiperitenone → cis-/trans-isopulegone → (+)-pulegone → (-)-menthone This pathway is highly regulated at the transcriptional and post-transcriptional levels, with pulegone reductase serving as a critical in piperita that determines the efficiency of menthone accumulation by reducing the C=C in pulegone. Yield of menthone is influenced by genetic variations among cultivars, such as differences in enzyme expression levels that alter pathway flux toward menthone versus or menthofuran. Environmental stressors, including high light intensity and cooler temperatures, promote menthone accumulation over by upregulating reductase activities and suppressing menthofuran formation, whereas low light and warm conditions favor the menthofuran branch. Recent research post-2020 has focused on to enhance menthone production, including overexpression of pathway genes like pulegone reductase using tissue-specific promoters, which has increased menthone levels by redirecting flux in transgenic lines. A 2023 study demonstrated that cyanobacterial elicitors upregulated menthone reductase by up to 65% in piperita, boosting yields and pathway efficiency in hybrid cultivars through metabolic priming.

Chemical Structure and Stereochemistry

Molecular Framework

Menthone is an classified as a monoterpenoid , with the molecular formula C₁₀H₁₈O and a of 154.25 g/mol. Its IUPAC name is 2-isopropyl-5-methylcyclohexan-1-one, reflecting the unsubstituted core structure without specifying . For the naturally predominant l-menthone , the systematic IUPAC name is (2S,5R)-5-methyl-2-(propan-2-yl)cyclohexan-1-one. The core molecular framework consists of a six-membered ring, featuring a functional group at 1, an isopropyl substituent at 2, and a at 5. This arrangement positions the as the defining feature, with the alkyl substituents providing the branched chain characteristic of menthane-derived compounds. The SMILES notation for the basic, non-stereospecific form is CC1CCC(C(C1=O)C(C)C)C, which encapsulates the ring and pendant groups. Infrared spectroscopy confirms the presence of the ketone moiety through the characteristic C=O stretching vibration at approximately 1715 cm⁻¹, typical for saturated cyclic ketones like menthone. Menthone serves as a key precursor to menthol, obtained via stereoselective reduction of the carbonyl group. The molecule possesses two chiral centers at C2 and C5, giving rise to stereoisomers, though the framework itself remains consistent across configurations.

Stereoisomers and Configurations

Menthone features two chiral centers located at the and positions of its ring, resulting in four possible stereoisomers. The trans-configured pair consists of (2S,5R)-menthone, commonly referred to as l-menthone, and its (2R,5S)-menthone, known as d-menthone. The cis-configured pair comprises (2S,5S)-isomenthone and (2R,5R)-isomenthone. The of l-menthone is [α]D20 = −20° (neat), while d-menthone exhibits +20° under similar conditions. In natural sources, the l-menthone predominates. Conformational analysis reveals that menthone adopts a conformation for its ring, with the isopropyl and methyl substituents preferentially occupying equatorial positions to minimize steric interactions. This structure is supported by broadband Fourier-transform , which identifies three low-energy conformers for menthone, all featuring equatorial substituents. Although direct crystallographic data for menthone itself is limited due to its liquid state at , studies on menthone derivatives confirm the chair motif with equatorial orientations. In equilibrated mixtures, menthone and isomenthone exist in an approximately 70:30 ratio favoring menthone, reflecting the lower energy of the configuration. This distribution arises from acid- or base-catalyzed epimerization at the C5 position and has been quantified through analysis of reaction endpoints. Computational modeling of energy minima, including calculations, aligns with these experimental ratios by predicting a thermodynamic preference for the isomer due to reduced 1,3-diaxial interactions in the chair form.

Physical and Sensory Properties

Thermodynamic and Physical Characteristics

Menthone appears as a colorless to pale yellow liquid at , exhibiting an oily and mobile consistency. Key physical properties include a of 0.895 g/cm³ at 20°C and a of 1.450. Its is -6°C, while the is 207°C at 760 mmHg, with a of approximately 0.3 mmHg at 20°C. These thermal characteristics indicate menthone's suitability for processes, where vapor-liquid equilibrium data for binary mixtures, such as with n-decane, have been established to model separation efficiency.
PropertyValueConditionsSource
Density0.895 g/cm³20°CPubChem
Refractive Index1.450-ChemicalBook
Melting Point-6°C-
Boiling Point207°C760 mmHg
Vapor Pressure~0.3 mmHg20°CRIFM
Menthone demonstrates low in , approximately 0.7 g/L at 25°C, rendering it effectively insoluble for practical purposes, though it is miscible with organic solvents such as , , and . Its is 73°C, highlighting moderate flammability risks during handling. The volatility of menthone, governed by its , contributes to its role in sensory applications through efficient .

Odor and Flavor Profiles

Menthone imparts a primary scent characterized as minty and cooling, accompanied by herbal, woody, and slightly fruity undertones. Its odor detection threshold in air is reported at ppb (0.17 ppm), enabling perception at low concentrations. Among its stereoisomers, l-menthone delivers an intense note with strong minty qualities. In contrast, d-isomenthone exhibits a more and green aroma profile, which is less pronounced in mintiness compared to l-menthone. In terms of flavor, menthone provides a sharp, cooling sensation reminiscent of but lacking the typical alcoholic bite, described as -like with fresh green, , and refreshing aftertastes at concentrations around 50 ppm. Sensory evaluations using gas chromatography-olfactometry (GC-O) highlight menthone's significant contribution to the overall aromatic profile of peppermint essential oil, where it enhances the minty and cooling attributes alongside major components like menthol.

Preparation and Synthesis

Extraction from Natural Sources

Menthone is extracted from natural sources primarily through steam distillation of leaves from peppermint (Mentha × piperita) or related mint species such as cornmint (Mentha arvensis). In this industrial process, chopped plant material is subjected to steam at temperatures around 100°C, which volatilizes the essential oils without degrading heat-sensitive components. The vapors are condensed, and the immiscible oil layer is separated from the hydrosol, yielding a crude essential oil that serves as the starting material for menthone isolation. The crude oil, which typically contains 10-20% menthone by weight depending on plant variety and harvest conditions, undergoes to concentrate menthone. This step separates components based on boiling points, with the menthone cut collected in the 200-210°C range under reduced pressure to minimize thermal exposure. is employed in this purification to prevent decomposition of menthone and related monoterpenoids, as higher temperatures under atmospheric conditions can lead to or oxidation. Yields of menthone from oil average 10-20% of the total oil content, influenced by factors like and efficiency. For higher purity, fractional isolates l-menthone by cooling the distilled fraction to approximately -20°C, promoting selective precipitation of crystals with over 95% enantiomeric purity. This method leverages the low of l-menthone (around -6°C) and its differential solubility in the oil matrix at subzero temperatures. Enantioselective separation of menthone isomers can be further refined using chiral , such as with cyclodextrin-based stationary phases, to achieve baseline of enantiomers for analytical or preparative purposes. As a modern alternative to traditional , supercritical CO₂ extraction offers higher selectivity for menthone and other lipophilic components, operating at pressures of 100-400 bar and temperatures of 40-60°C to yield oils with reduced thermal artifacts and improved purity. This solvent-free method extracts up to 3.7% oil from leaves, preserving higher proportions of menthone compared to processes, and has been advanced in recent patents and studies for scalable industrial application.

Laboratory and Industrial Synthesis

Menthone is classically synthesized in the laboratory through the oxidation of using chromic acid-based reagents, such as the Jones reagent ( in and acetone), which selectively oxidizes the secondary group to a with yields typically ranging from 80% to 90%. This method, while effective, carries a risk of , particularly when starting from enantiopure , due to the acidic conditions that can lead to enolization and loss of stereochemical integrity. An alternative laboratory route involves the catalytic of pulegone, often derived from , using (Pd/C) as the catalyst under mild conditions, achieving stereoselective formation of (-)-menthone with selectivities up to 86% in isomer mixtures favoring menthone over isomenthone. This approach benefits from pulegone's availability as a natural precursor and allows control over through catalyst selection, though heterogeneous catalysts like Pd/C may produce mixtures requiring separation. Modern laboratory syntheses emphasize sustainability and , including biocatalytic reduction of pulegone using pulegone reductase enzymes, such as the newly characterized bacterial pulegone reductase (PGR) reported in 2024, which exhibits high catalytic efficiency (k_cat/K_M > 10^5 M^{-1} s^{-1}) and enables enantiopure (-)-menthone when enzymes are immobilized for reuse in flow systems. Additionally, asymmetric syntheses from acyclic precursors like , involving chiral catalysis and cyclization as in adaptations of the Takasago menthol process, provide scalable routes to enantiopure menthone intermediates with overall yields exceeding 70% and enantiomeric excess >99%. Recent 2025 advancements include lipase-based enzymatic resolutions for synthesis pathways involving menthone. On an industrial scale, menthone is produced in multi-ton quantities primarily through upgrading of peppermint oil fractions, where excess pulegone or from natural extracts is hydrogenated or oxidized to menthone using heterogeneous catalysts like or , integrating into larger menthol production streams. Racemic menthone is economically viable at approximately $10 per kg due to simple catalytic processes, while enantiopure variants command prices around $100 per kg owing to the need for chiral catalysts or enzymatic resolutions in purification steps. These methods ensure high-purity menthone for and fragrance applications, often achieving >90% purity post-distillation.

Chemical Reactivity and Derivatives

Key Reaction Mechanisms

Menthone, as a cyclic , exhibits characteristic reactivity at its toward . Grignard reagents, such as , add to the carbonyl carbon of menthone, forming a tetrahedral that, upon acidic , yields a tertiary alcohol like 1-phenylmenthol. This reaction follows the standard mechanism for ketones, where the nucleophilic carbon of the organomagnesium species attacks the electrophilic carbonyl, displacing the to generate the . The carbonyl can also undergo stereoselective reduction with (NaBH₄) in protic solvents like or , yielding a mixture of (-)- and (+)-neomenthol as diastereomers, with menthol typically the major product through equatorial delivery in the conformation of menthone and neomenthol from axial . Ratios vary with solvent and conditions but often favor menthol (around 60–80% menthol to 20–40% neomenthol), highlighting steric control in the . Epimerization of menthone at the alpha position occurs under base-catalyzed conditions via to form the , which protonates on the opposite face to yield isomenthone, establishing an governed by the relative thermodynamic stabilities of the diastereomers. The K = \frac{[\text{isomenthone}]}{[\text{menthone}]} \approx 0.43 at 25°C in alcoholic solvents, favoring menthone due to its more stable . In the Baeyer-Villiger oxidation, menthone reacts with peracids like m-chloroperoxybenzoic acid (mCPBA) to insert an oxygen atom adjacent to the carbonyl, forming a δ-valerolactone derivative. The mechanism involves nucleophilic addition of the peracid to the carbonyl, followed by migration of the more substituted alkyl group—the carbon bearing the isopropyl substituent—due to its higher migratory aptitude compared to the unsubstituted methylene group, ensuring regioselectivity. This reaction, first demonstrated on menthone in 1899, proceeds with retention of configuration at the migrating carbon. Menthone participates in aldol condensations, particularly with aromatic s under basic conditions, via Claisen-Schmidt mechanisms where the from menthone's alpha carbon attacks the carbonyl, followed by to an α,β-unsaturated . These reactions are facilitated by the hindered nature of menthone, requiring strong bases like tert-butoxide for efficient formation, and yield E-configured products with high .

Common Derivatives

Menthyl acetate is a prominent derivative in the menthane series, formed indirectly from menthone through selective reduction to followed by esterification with or under mild conditions, typically yielding the with high efficiency. This compound possesses the molecular formula C₁₂H₂₂O₂ and is characterized by its clear, colorless liquid state at , with a mild, fruity-minty that distinguishes it from the sharper profile of menthone itself. Pulegone represents an oxidized derivative of menthone, accessible via dehydrogenation reactions that introduce an exocyclic , although such transformations are less prevalent than the biosynthetic reduction of pulegone to menthone. With the C₁₀H₁₆O, pulegone is a pale yellow liquid featuring a pungent, minty aroma and is notably hepatotoxic, prompting regulatory limits in and applications due to its potential to form reactive metabolites like menthofuran. 8-Hydroxymenthone emerges from oxidation of menthone, often as an intermediate in metabolic or synthetic pathways involving enzymatic systems, resulting in a hydroxyl group at the 8-position of the isopropyl . The compound, C₁₀H₁₈O₂, appears as a metabolite in studies of transformations and displays increased polarity due to the secondary functionality, influencing its solubility and further reactivity. Recent advancements have highlighted menthone-derived compounds as chiral ligands in asymmetric catalysis; for instance, diastereoselective addition of organolithium reagents to (-)-menthone yields aminoalcohol derivatives that coordinate with in the enantioselective ethylation of aldehydes, achieving up to 80% enantiomeric excess. These ligands, featuring or heteroatoms appended to the menthane skeleton, leverage the inherent of menthone for high stereocontrol in carbon-carbon bond formations. In 2023, biocatalytic of menthone produced neomenthylamine derivatives, expanding their utility in design for pharmaceutical synthesis.

Applications and Biological Activity

Industrial and Commercial Uses

Menthone serves as a key agent in the and oral care industries, imparting a characteristic minty taste to products such as , , and candies. It is typically incorporated at usage levels up to 1,000 ppm, enhancing the refreshing profile of synthetic and formulations. The U.S. recognizes menthone as (GRAS) for use as a direct in , supporting its widespread application in these consumer goods. Its minty flavor profile, derived from natural occurrences in and related essential oils, makes it a preferred component for achieving desired sensory attributes without overpowering other ingredients. In the fragrance sector, menthone functions as a versatile ingredient in perfumes, soaps, and , where it provides a cool, minty top note that adds lift and freshness even at low concentrations. This diffusive, peppermint-like aroma contributes to the overall composition in trace amounts, blending well with floral and herbal accords to create balanced scents. Its role in these applications is supported by its natural presence in mint oils, allowing for formulations that mimic botanical freshness in commercial and items. Beyond flavor and fragrance, menthone acts as an important precursor in the industrial of , undergoing or stereospecific to yield the , which is essential for larger-scale production of mint-derived compounds. Additionally, menthone exhibits insecticidal properties, finding emerging use in natural pesticides as a component of plant-based formulations targeting stored pests like the . The global menthone market, driven by demand for natural mint alternatives in these sectors, was valued at USD 177.1 million in 2024 and is projected to reach USD 265.2 million by 2033.

Pharmacological Properties and Toxicity

Menthone exhibits pharmacological activity primarily through activation of the transient receptor potential melastatin 8 (TRPM8) ion channel, which contributes to a cooling sensation upon topical application, though less potently than menthol. This activation occurs at concentrations requiring higher levels compared to menthol, facilitating its use in imparting mild cooling effects in various formulations. Additionally, menthone demonstrates anti-inflammatory properties by inhibiting the secretion of proinflammatory cytokines such as TNF-α in lipopolysaccharide-stimulated lung mast cells at concentrations ranging from 0.5 to 50 μM. In terms of therapeutic potential, menthone shows antimicrobial activity against methicillin-resistant Staphylococcus aureus (MRSA), with a (MIC) of 3.54 mg/mL and a (MBC) of 7.08 mg/mL, attributed to membrane damage and alterations in the . It also possesses general neuroprotective effects, including activity that may protect against neuronal damage, as evidenced in studies on monoterpenes. While not specifically tied to Alzheimer's models in recent literature, its neuroprotective profile supports further investigation for neurodegenerative applications. effects are implied through its TRPM8-mediated cooling, which can provide counterirritant relief in topical contexts, though direct clinical use in creams is more commonly associated with menthol derivatives. Regarding toxicity, menthone has low acute oral toxicity in rats, with an LD50 value of approximately 2,000 mg/kg, indicating minimal from single exposures at typical doses. It acts as a and eye irritant, causing serious eye damage and mild to moderate irritation upon direct contact, but shows no evidence of carcinogenicity and is unclassified by the International Agency for Research on Cancer (IARC). Inhalation studies are limited, but no severe respiratory has been reported at low exposures; however, high concentrations may cause similar to other monoterpenes. Menthone is registered under the Union's REACH regulation, confirming its approval for industrial and commercial use with appropriate safety assessments.

Historical Development

Discovery and Early Synthesis

Menthone's discovery occurred amid the late 19th-century surge in chemistry, driven by chemists like Otto Wallach who systematically investigated the structures and transformations of volatile compounds from essential oils, laying the foundations for understanding monoterpenoids. This era saw rapid advancements in isolating and synthesizing from natural sources such as and , fueled by improved and oxidation techniques, though menthone itself was not isolated from nature until the 1890s despite its presence as a minor component in oils like . The compound was first synthesized in 1881 by M. Moriya at the through the oxidation of using a mixture at elevated temperatures around 120°C, yielding menthone as a derivative and marking one of the earliest targeted syntheses in chemistry. This synthetic route highlighted menthone's relationship to , a major constituent of oil, and provided the initial pure samples for further study, predating its natural isolation. Early investigations into menthone's were advanced in 1889 by Ernst Beckmann, who observed changes in upon treating menthone with concentrated , leading to the discovery of its epimerization to isomenthone—a process that interconverts the cis and trans isomers at the C-5 position and demonstrated the compound's configurational lability under acidic conditions. Building on this, Beckmann detected menthone as a natural component in oil in 1891 through careful and analysis, confirming its occurrence alongside . The structure was proposed in 1900 by Otto Wallach via degradative methods, including and oxidation, which broke down menthone to identifiable fragments like acetic and isopropylacetic acids, solidifying its identity as 5-methyl-2-(1-methylethyl) within the family.

Key Scientific Advancements

The of menthone was first achieved in 1881 by M. Moriya at the , who oxidized with to produce the , marking an early milestone in chemistry. This synthetic route preceded its natural isolation from oil, which was reported in 1891 by Ernst Beckmann. These developments laid the foundation for understanding menthone's role in mint-derived compounds, shifting focus from empirical extraction to controlled chemical manipulation. A pivotal advancement came in 1899 when and Victor Villiger employed menthone as a key substrate in their discovery of the Baeyer-Villiger oxidation, using Caro's reagent () to convert the cyclic into the corresponding , mentholactone. This , which inserts an oxygen atom adjacent to the , revolutionized by providing a general method for and formation from ketones, with menthone exemplifying its utility on unsymmetrical substrates. The mechanism, later elucidated through migratory aptitude studies, remains a cornerstone of synthetic methodology, influencing applications from pharmaceuticals to polymers. In the mid-20th century, menthone gained prominence in industrial processes for production, notably through the Bouveault-Blanc reduction, where sodium in converted menthone-isomenthone mixtures to , enabling scalable aroma chemical manufacturing by the . This was further advanced in the 1970s by Haarmann & Reimer (now ), who developed enantioselective syntheses starting from or , incorporating menthone as an intermediate to produce high-purity (-)-, addressing supply shortages from natural sources. Biosynthetic insights emerged in the late 20th and early 21st centuries, with the cloning and characterization of enzymes catalyzing menthone formation and reduction. In 2001, researchers cloned menthofuran synthase, revealing menthone's role in glandular trichome , while 2005 studies cloned (-)-menthone:(-)- reductase and (+)-menthone:(+)-neomenthol reductase, accounting for stereospecific composition in × piperita. These genetic advancements enabled for enhanced yields. Recent high-impact research has uncovered menthone's pharmacological potential, including its 2023 elucidation as a potent against (MRSA) via membrane disruption and inhibition, with minimum inhibitory concentrations as low as 0.25 mg/mL. Additionally, a 2022 study demonstrated menthone's regulation of T-cell subtypes to alleviate collagen-induced in mice, reducing pro-inflammatory cytokines like IL-17 by up to 50%, highlighting its therapeutic promise.

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