Method for synthesizing carvone

Abstract

The invention discloses a perfume synthesis method in the technical field of chemical industry, in particular relates to a method for synthesizing carvone by taking epoxy limonene as a raw material. The method comprises the following steps of: taking the epoxy limonene, zinc caprylate and 2-aminophenol as raw materials; performing an isomerization reaction on the epoxy limonene under the action of a catalyst to obtain carveol; and oxidizing the carveol to obtain the carvone. The method has the advantages of economic and environmental-friendly synthesis technology, no production of sewage, capability of avoiding the production of a large amount of waste water which has high organic matter content and is difficult for biodegradation and oxygenolysis in the conventional process, capability of recycling the catalyst, simple and readily available raw materials, short reaction time, high conversion rate, high selectivity and suitability for industrial production.

Description

technical field

[0001] The invention relates to a chemical synthesis method, in particular to a synthesis method of spices and spices. technical background

[0002] Carvone (Carvone) scientific name is 1-methyl 4-isopropenyl-6-cyclohexen-2-one, English name: 2-Methyl-5-isopropenyl-2-cyclohexen-1-one. Carvone is the main component of spearmint. It has a strong spearmint smell. It has a sweet, soft and powerful aroma. It is widely used in toothpaste, chewing gum, gummies and other sugar foods. It is also commonly used in violets. Type, sweet-scented osmanthus, jasmine and other flavors. It can also be used as a high-efficiency solvent in industry. Carvone has now become a bulk spice, with an annual output of more than 2,000 tons.

[0003] At present, there are mainly two types of carvone, natural and synthetic. Carvone extracted from natural essential oils has the disadvantages of small output and high price, and is limited by natural conditions and seasons, so it cannot m...

Examples

Embodiment 1

[0022] In a 100 ml three-necked flask, add 50.0 grams of epoxy limonene (content 97%), 0.4 grams of 2-aminophenol (n / n: 86:1), stir with a magnetic stirrer, and heat to an internal temperature of 180 to 190 °C, after 4-6 hours, the rearrangement reaction was completed, and 46.7 g of crude carveol was obtained by distillation under reduced pressure, and then the finished product of carveol was obtained after rectification. The conversion rate of epoxylimonene was 85%, and the selectivity of carveol was 89%.

Embodiment 2

[0024] In a 100 ml three-necked flask, add 50.0 grams of limonene epoxy (content 97%), 2.1 grams of zinc octoate (n / n: 86:1), stir with a magnetic stirrer, and heat to an internal temperature of 180 to 190 ° C. After 4 to 6 hours, the rearrangement reaction was completed, and 42.3 g of crude carveol was obtained by distillation under reduced pressure, and the finished product of carveol was obtained after rectification. The conversion rate of epoxylimonene was 85.8%, and the selectivity of carveol was 81.2%.

Embodiment 3

[0026] In a 100 ml three-necked flask, add 50.0 g of limonene epoxy (content 97%) and 1.53 g of zinc octoate (n / n: 63:1), stir with a magnetic stirrer, and heat to an internal temperature of 205-210°C. After 4 to 6 hours, the rearrangement reaction was completed, and 43.7 g of crude carveol was obtained by distillation under reduced pressure, and the finished product of carveol was obtained after rectification. The conversion rate of epoxylimonene was 87.1%, and the selectivity of carveol was 83.1%.

technical field

[0001] The invention relates to a chemical synthesis method, in particular to a synthesis method of spices and spices. technical background

[0002] Carvone (Carvone) scientific name is 1-methyl 4-isopropenyl-6-cyclohexen-2-one, English name: 2-Methyl-5-isopropenyl-2-cyclohexen-1-one. Carvone is the main component of spearmint. It has a strong spearmint smell. It has a sweet, soft and powerful aroma. It is widely used in toothpaste, chewing gum, gummies and other sugar foods. It is also commonly used in violets. Type, sweet-scented osmanthus, jasmine and other flavors. It can also be used as a high-efficiency solvent in industry. Carvone has now become a bulk spice, with an annual output of more than 2,000 tons.

[0003] At present, there are mainly two types of carvone, natural and synthetic. Carvone extracted from natural essential oils has the disadvantages of small output and high price, and is limited by natural conditions and seasons, so it cannot m...

Examples

Embodiment 1

[0022] In a 100 ml three-necked flask, add 50.0 grams of epoxy limonene (content 97%), 0.4 grams of 2-aminophenol (n / n: 86:1), stir with a magnetic stirrer, and heat to an internal temperature of 180 to 190 °C, after 4-6 hours, the rearrangement reaction was completed, and 46.7 g of crude carveol was obtained by distillation under reduced pressure, and then the finished product of carveol was obtained after rectification. The conversion rate of epoxylimonene was 85%, and the selectivity of carveol was 89%.

Embodiment 2

[0024] In a 100 ml three-necked flask, add 50.0 grams of limonene epoxy (content 97%), 2.1 grams of zinc octoate (n / n: 86:1), stir with a magnetic stirrer, and heat to an internal temperature of 180 to 190 ° C. After 4 to 6 hours, the rearrangement reaction was completed, and 42.3 g of crude carveol was obtained by distillation under reduced pressure, and the finished product of carveol was obtained after rectification. The conversion rate of epoxylimonene was 85.8%, and the selectivity of carveol was 81.2%.

Embodiment 3

[0026] In a 100 ml three-necked flask, add 50.0 g of limonene epoxy (content 97%) and 1.53 g of zinc octoate (n / n: 63:1), stir with a magnetic stirrer, and heat to an internal temperature of 205-210°C. After 4 to 6 hours, the rearrangement reaction was completed, and 43.7 g of crude carveol was obtained by distillation under reduced pressure, and the finished product of carveol was obtained after rectification. The conversion rate of epoxylimonene was 87.1%, and the selectivity of carveol was 83.1%.

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