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Preparation method of Phantolide

A technology of powdered sandalwood musk and aluminum trichloride, which is applied in the field of preparation of powdered sandalwood musk, can solve the problems of difficulty in applying mass production, affecting the health of workers, and the high price of tert-amyl alcohol raw materials, so as to be beneficial to mass production and Promotion, reduction of raw material cost and labor cost, easy control effect

Pending Publication Date: 2021-09-10
安徽瑞邦香料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The raw material price of tert-amyl alcohol is high, and it is difficult to apply it in mass production in terms of production cost
[0004] The productivity of the above-mentioned prior art is low, and the utilization rate of atoms is not high, resulting in a waste of resources, and some processes use sulfuric acid equipment to corrode seriously
The production process adopts intermittent production technology, which requires front-line workers to frequently load and discharge materials in each process, which is labor-intensive, easily affects the health of workers, and is easy to introduce impurities, and some volatile substances are easy to leak into the air, which is harmful to safe production. Unfavorable operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Mix 2 parts of aluminum trichloride with 1.5 parts of triethylamine hydrochloride, and react at 105°C for 0.5 h to prepare an aluminum trichloride ionic liquid.

[0029] (2) Mix 1 part of p-cymene and 0.6 part of isopentene in a stirred tank to obtain a raw material mixture.

[0030] (3) According to the weight ratio of 25:1, add the mixed solution and the aluminum trichloride ionic liquid dropwise into the continuous reaction kettle with the upper outlet at the same time, control the reaction temperature at 15°C, stir, and stay in the reaction kettle for 1h Finally, the reaction liquid is obtained from the discharge port.

[0031] (4) The obtained reaction solution is washed with water and the raw materials are recovered to obtain the crude intermediate.

[0032] (5) Take 2 parts of the intermediate crude product and 1 part of acetyl chloride in 3.5 parts of dichloroethane solvent, add 1.5 parts of aluminum trichloride to carry out acylation reaction, obtain the p...

Embodiment 2

[0034] (1) Mix 2 parts of aluminum trichloride with 1.05 parts of triethylamine hydrochloride, and react at 125°C for 2 hours to prepare an aluminum trichloride ionic liquid.

[0035] (2) Mix 1 part of p-cymene and 1 part of isopentene in a stirred tank to obtain a raw material mixture.

[0036] (3) According to the weight ratio of 20:1, add the mixed solution and the aluminum trichloride ionic liquid dropwise into the continuous reaction kettle with the upper outlet at the same time, control the reaction temperature at 15°C, stir, and stay in the reaction kettle for 1h Finally, the reaction liquid is obtained from the discharge port.

[0037] (4) The obtained reaction solution is washed with water and the raw materials are recovered to obtain the crude intermediate.

[0038] (5) Take 2 parts of intermediate crude product and 1 part of acetyl chloride in 3.5 parts of dichloromethane solvent, add 1.5 parts of aluminum trichloride to carry out acylation reaction, obtain powdery...

Embodiment 3

[0040] (1) Mix 2 parts of aluminum trichloride with 1.2 parts of triethylamine hydrochloride, and react at 150°C for 1 hour to prepare an aluminum trichloride ionic liquid.

[0041] (2) Mix 1 part of p-cymene and 1.5 parts of isopentene in a stirred tank to obtain a raw material mixture.

[0042] (3) According to the weight ratio of 15:1, add the mixed solution and the aluminum trichloride ionic liquid dropwise into the continuous reaction kettle with the upper outlet at the same time, control the reaction temperature at 0°C, stir, and stay in the reaction kettle for 1h Finally, the reaction liquid is obtained from the discharge port.

[0043] (4) The obtained reaction solution is washed with water and the raw materials are recovered to obtain the crude intermediate.

[0044] (5) Take 2 parts of the intermediate crude product and 1 part of acetyl chloride in 3.5 parts of cyclohexane solvent, add 1.5 parts of aluminum trichloride to carry out acylation reaction, and obtain the...

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PUM

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Abstract

The invention belongs to the field of organic synthesis, and particularly relates to a preparation method of Phantolide, which adopts ionic liquid as a catalyst, and adopts p-isopropyltoluene and isoamylene as raw materials for continuous production. The preparation method provided by the invention improves the total yield of Phantolide products, the production is continuous and easy to control, and the labor intensity of workers is greatly reduced.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a method for preparing sandalwood musk. Background technique [0002] In the prior art, p-cymene and isopentene are generally used as raw materials, anhydrous aluminum trichloride is used as a catalyst, the reaction is carried out at a certain temperature and then rectified under reduced pressure to obtain intermediates 1, 1, 2, 3, 3 , 6-hexamethylindane, and then 1,1,2,3,3,6-hexamethylindane and acetyl chloride in a solvent, adding aluminum trichloride catalyst for acylation reaction, and then refining under reduced pressure Distillation obtains the final product powder sandalwood musk. [0003] It is also reported that the use of tert-amyl alcohol, p-cymene, and sulfuric acid is used as a catalyst for the synthesis of intermediates, and the second step is the same. The raw material price of tert-amyl alcohol is high, and in terms of production cost, it is difficul...

Claims

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Application Information

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IPC IPC(8): C07C45/46C07C49/792C07C2/72C07C13/48
CPCC07C45/46C07C2/72C07C2527/126C07C2602/10C07C13/48C07C49/792Y02P20/584
Inventor 孙伟张小锋王俊
Owner 安徽瑞邦香料有限公司
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