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A kind of preparation method of blackwood alcohol

A technology of sagebyl alcohol and sec-butanol, which is applied in the field of preparation of sagebyl alcohol, can solve problems such as reducing product yield, and achieve the effects of improving selectivity, increasing reaction yield, and high yield

Active Publication Date: 2021-03-12
江苏馨瑞香料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The two-step reaction of this patent uses sodium methoxide and sodium borohydride as catalysts respectively. Although the reaction conditions are mild, it needs to be washed with water during the reaction process, and the product is extracted with toluene, which produces a large amount of waste water and reduces the yield of the product.

Method used

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  • A kind of preparation method of blackwood alcohol
  • A kind of preparation method of blackwood alcohol

Examples

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Embodiment 1

[0017] A preparation method of sagelic alcohol, comprising step 1: putting 20 g of zinc bromide into 1500 g of toluene, adding 650 g of santalone dropwise into the reaction system, so that the temperature of the reaction system is maintained at 53-110° C., dropping After the addition, the reaction was continued for 5 minutes, and a sample was taken, and the content of santalone was analyzed by liquid chromatography to be 0.13%, and the first step reaction was completed. After recovering toluene by vacuum distillation of the reaction system in step 1, put 800g of sec-butanol and 80g of aluminum sec-butoxide, the reaction temperature is controlled at 100-125°C, and the reflux reaction is carried out in stages: 0-2h, the reaction temperature is controlled at 100-105°C , the temperature at the end of the reflux tube is controlled at ≦78°C, and methyl ethyl ketone is recovered while reacting; in the second hour to 3h, the reaction temperature is controlled at 105-115°C, and the temp...

Embodiment 2

[0019] A method for preparing sagelic alcohol, comprising step 1: putting 20g of zinc bromide into 2500g of toluene, adding dropwise 650g of santalone into the toluene, maintaining the temperature of the reaction system at 57-98°C, and finishing the dropping Afterwards, continue to react for half an hour, take a sample, and the chromatographic analysis shows that the content of santalone is 0.11%, and the first step of reaction is completed. After recovering toluene by vacuum distillation of the reaction system in step 1, put in 1500g of sec-butanol and 80g of aluminum sec-butoxide, the reaction temperature is controlled at 100-125°C, and the reflux reaction is carried out in stages: 0-2h, the reaction temperature is controlled at 100-105°C , the temperature at the end of the reflux tube is controlled at ≦78°C, and methyl ethyl ketone is recovered while reacting; the reaction temperature is controlled at 105-115°C during the 2h-3h, and the temperature at the end of the reflux t...

Embodiment 3

[0021] A method for preparing sagelic alcohol, comprising step 1: putting 20g of zinc bromide into 2000g of toluene, adding dropwise 650g of santalone into the reaction system, maintaining the temperature of the reaction system at 65-100°C, adding dropwise After the end, continue to react for half an hour, take a sample, and analyze the content of santalone by liquid chromatography to be 0.08%, and the first step reaction ends. After recovering toluene by vacuum distillation of the reaction system in step 1, put 800g of sec-butanol and 80g of aluminum sec-butoxide, the reaction temperature is controlled at 100-125°C, and the reflux reaction is carried out in stages: 0-2h, the reaction temperature is controlled at 100-105°C , the temperature at the end of the reflux tube is controlled at ≦78°C, and methyl ethyl ketone is recovered while reacting; in the second hour to 3h, the reaction temperature is controlled at 105-115°C, and the temperature at the end of the reflux tube is co...

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Abstract

The invention provides a preparation method of ebony alcohol, comprising the following steps. Step 1: under the catalysis of zinc bromide, santalone is subjected to isomerization reaction; step 2: in step 1, the reaction product and sec-butanol are Under the catalysis of aluminum sec-butoxide, ebony alcohol is generated. The preparation method of ebony alcohol has the advantages of environmental protection and high yield.

Description

technical field [0001] The present invention relates to a kind of preparation method of blackwood alcohol. Background technique [0002] The Chinese alias of ebony alcohol is 3-methyl-5-(2,2,3-trimethyl-3-cyclopenten-1-yl)-4-penten-2-ol, which is not only rich in The natural sandalwood aroma is strong and penetrating. It is mainly used in the formulation of woody-scented daily chemical essence. It can make the aroma of the essence more full and has a diffuse sandalwood aroma. [0003] The preparation method of ebony alcohol mainly includes condensation with 2-butanone using borneolein as raw material, and then isomerizing the condensation product with potassium tert-butoxide in dimethylformamide, so that the double bond is translocated, Finally, reduction with sodium borohydride gave a mixture of four diastereoisomers. The preparation method of patent CN103483151A ebony alcohol discloses that methyl ethyl ketone and borneolenal are used as initial raw materials, and the pr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C33/12C07C29/143
CPCC07C29/143C07C45/67C07C2601/10C07C49/21C07C33/12
Inventor 应登宇陈伟应思斌刘洋赵健标
Owner 江苏馨瑞香料有限公司
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