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Method for preparing spice of Cashmeran

A technology of cashmerone and spices, applied in the field of preparation of spices cashmerone, can solve problems such as inability to meet market demand, achieve high social use value and application prospects, reduce pollution, and achieve high economic benefits

Active Publication Date: 2022-01-14
安徽金禾化学材料研究所有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the current production processes have their own shortcomings and cannot meet market demand.

Method used

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  • Method for preparing spice of Cashmeran
  • Method for preparing spice of Cashmeran

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] A method for preparing spice cashmerone, comprising the following steps:

[0038] S1: Hydrogenation to get 1,1,2,3,3-pentamethyl-4,5,6,7-tetrahydroindan

[0039] Add 300g of 1,1,2,3,3-pentamethylindane and 3g of palladium carbon into the reaction kettle, first blow through 0.4Mpa nitrogen three times to remove the air in the reaction kettle; then pass through 0.35Mpa hydrogen three times to remove Nitrogen in the reaction kettle; feed 1.5Mpa hydrogen, heat up to 130°C, and then replenish hydrogen until the hydrogen pressure is 3Mpa, react at this pressure and temperature for 9 hours, and the obtained products are mainly 1, 1, 2, 3, The mixture of 3-pentamethyl-4,5,6,7-tetrahydroindan was 290 g, and the purity was 63%.

[0040] S2: Oxidation to get cashmerone

[0041] Put all the 1,1,2,3,3-pentamethyl-4,5,6,7-tetrahydroindane obtained by hydrogenation with a purity of 63% into the reaction kettle, add 600g of ACN as a solvent, and then add the catalyst nitric acid Iro...

Embodiment 2

[0043] A method for preparing spice cashmerone, comprising the following steps:

[0044] S1: Hydrogenation to get 1,1,2,3,3-pentamethyl-4,5,6,7-tetrahydroindan

[0045]Add 300g of 1,1,2,3,3-pentamethylindane and 3g of palladium carbon into the reaction kettle, first pass through 0.3Mpa nitrogen for three times to remove the air in the reaction kettle; then pass through 0.4Mpa hydrogen for three times to remove Nitrogen in the reaction kettle; feed 2Mpa hydrogen, heat up to 130°C, and then replenish hydrogen until the hydrogen pressure is 3Mpa, react at this pressure and temperature for 16 hours, and the obtained products are mainly 1, 1, 2, 3, 3 - The mixture of pentamethyl-4,5,6,7-tetrahydroindane is 300 g with a purity of 65%.

[0046] S2: Oxidation to get cashmerone

[0047] Put all the 1,1,2,3,3-pentamethyl-4,5,6,7-tetrahydroindane obtained by hydrogenation with a purity of 65% into the reaction kettle, add 600g of ACN as a solvent, and then add the catalyst Zinc nitrat...

Embodiment 3

[0049] A method for preparing spice cashmerone, comprising the following steps:

[0050] S1: Hydrogenation to get 1,1,2,3,3-pentamethyl-4,5,6,7-tetrahydroindan

[0051] Add 600g of 1,1,2,3,3-pentamethylindane and 3g of palladium carbon into the reaction kettle, first pass through 0.3Mpa nitrogen for three times to remove the air in the reaction kettle; then pass through 0.4Mpa hydrogen for three times to remove Nitrogen in the reactor. Introduce 2Mpa of hydrogen, heat up to 140°C, then add hydrogen until the pressure of hydrogen is 3Mpa, react at this pressure and temperature for 14 hours, and the main product is 1,1,2,3,3-pentamethyl-4 , The mixture of 5,6,7-tetrahydroindane was 600g, and the purity was 64%.

[0052] S2: Oxidation to get cashmerone

[0053] Put 600g of 1,1,2,3,3-pentamethyl-4,5,6,7-tetrahydroindane obtained by hydrogenation with a purity of 64% into the reaction kettle, add 600g of ACN as a solvent, and then add the catalyst Copper nitrate and 2,2,6,6-tet...

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Abstract

The invention relates to the technical field of chemical engineering, and in particular, relates to a method for preparing spice of Cashmeran, wherein the method comprises the following steps: S1: 1, carrying out catalytic hydrogenation on 1,1,2,3,3-pentamethylindane through a palladium catalyst, a nickel catalyst, a copper-zinc catalyst, a cobalt catalyst, a Pt catalyst, a ruthenium catalyst and the like to obtain 1,1,2,3,3-pentamethyl-4,5,6,7-tetrahydroindane, and S2, introducing oxygen or a mixed gas of oxygen and air into the 1,1,2,3,3-pentamethyl-4,5,6,7-tetrahydroindane, and carrying out oxidation under the action of a catalyst A and a catalyst B so as to generate the Cashmeran. According to the method, a chromium-containing oxidant is not used, so that the pollution is reduced, and meanwhile, the energy consumption is reduced and the production cost is reduced due to mild reaction conditions.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a method for preparing spice cashmerone. Background technique [0002] Cashmerone [chemical name 1,1,2,3,3-pentamethyl-6,7-dihydro-4(5H)indanone], also referred to as indanone, is an organic substance with a light yellow liquid appearance. It has a strong musk, floral and ambergris flavor. It is the raw material for the preparation of high-end perfumes and cosmetic essences, and is especially favored by perfumers. A kind of musk fragrance compound successfully researched by the American International Fragrance Company (I.F.F.) in the 1970s. [0003] IFF company first developed and reported the synthetic route of cashmerone and published it in patent 3876562. Its hydrogenation stage uses Raney nickel as catalyst, 1000psi pressure, hydrogenation at 150-185℃, potassium dichromate for oxidation As a catalyst, cashmerone can be obtained. However, this solution has high...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/34C07C49/633C11B9/00B01J31/02
CPCC07C45/34C07C5/11C11B9/0049B01J27/25B01J31/0271B01J31/0247C07C2602/08B01J2231/70C07C49/633C07C13/465
Inventor 方茂海杨志健石雅义李亚玲梁峰
Owner 安徽金禾化学材料研究所有限公司
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