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Synthesis method of 3-methyl-2-butyl mercaptan

A synthesis method and technology of butanethiol, applied in the field of flavors and fragrances, can solve the problems of low extraction rate, oxidation side reactions, etc., and achieve the effects of reducing reaction temperature, improving yield and optimizing reaction environment

Pending Publication Date: 2022-02-11
河南蔚源生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The thiotal / ketonization reaction of thiols with carbonyl compounds is a common method for protecting functional groups, and it is important and widely used in multi-step synthesis or synthesis of natural products. 3-Methyl-2-butanethiol is a A kind of meat-flavored spice with elegant aroma and good natural feeling. It is widely used in the configuration of flavors and fragrances. In the current extraction process, the reaction temperature is too high, and oxidation side reactions are prone to occur during hydrolysis, and the extraction rate is low.

Method used

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  • Synthesis method of 3-methyl-2-butyl mercaptan
  • Synthesis method of 3-methyl-2-butyl mercaptan
  • Synthesis method of 3-methyl-2-butyl mercaptan

Examples

Experimental program
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Effect test

Embodiment 1

[0021] A kind of synthetic method of 3-methyl-2-butanethiol, its synthetic steps are as follows:

[0022] S1: Take 10 parts of tert-amyl alcohol and 1 part of concentrated sulfuric acid in parts by weight, first add tert-amyl alcohol into the volumetric flask, then slowly add concentrated sulfuric acid, stir and mix for 1 hour, and heat to 70 degrees, and continue to heat to 80 degrees , a dehydration reaction occurs, during which the liquid is distilled until the distilled liquid stops;

[0023] In the distilled liquid, add the sodium bicarbonate solution that is 0.7 parts by weight, stir for 5 minutes, let stand for 1 hour to separate layers, and the main components of the product are trimethylethylene, isomers and a small amount of tert-amyl alcohol at this time ;

[0024] S2: Use a 1.2m-long rectification column and a glass spring packing to rectify the distilled liquid obtained from S1, and collect the fraction at 30 degrees. In this temperature range, the isomers begin ...

Embodiment 2

[0033] A kind of synthetic method of 3-methyl-2-butanethiol, its synthetic steps are as follows:

[0034] S1: Take 8 parts of tert-amyl alcohol and 1 part of concentrated sulfuric acid by weight, first add tert-amyl alcohol into the volumetric flask, then slowly add concentrated sulfuric acid, stir for 1.5 hours, heat to 75 degrees, and continue to heat to 85 degrees, Dehydration reactions, in which liquid is distilled off until the distilling of liquid ceases;

[0035] In the distilled liquid, add the sodium bicarbonate solution that is 0.5 parts by weight, stir for 15 minutes, and let stand for 2.5 hours to separate layers. At this time, the main components of the product are trimethylethylene, isomers and a small amount of tert-amyl alcohol ;

[0036] S2: Use a 1.2m-long rectification column and a glass spring packing to rectify the distilled liquid obtained from S1, and collect the fraction at 35 degrees. Under this temperature range, the isomers begin to evaporate and di...

Embodiment 3

[0045] A kind of synthetic method of 3-methyl-2-butanethiol, its synthetic steps are as follows:

[0046] S1: Take 12 parts of tert-amyl alcohol and 1.5 parts of concentrated sulfuric acid by weight, first add tert-amyl alcohol into the volumetric flask, then slowly add concentrated sulfuric acid, stir for 2 hours, heat to 80 degrees, and continue to heat to 85 degrees, A dehydration reaction in which liquid is distilled off; until the distilling of liquid ceases;

[0047] In the distilled liquid, add the sodium bicarbonate solution that is 0.8 part by weight, stir for 10 minutes, leave standstill for 1.5 hours to separate layers, the main components of the product are trimethylethylene, isomers and a small amount of tert-amyl alcohol at this time ;

[0048]S2: Use a 1.2m-long rectification column and a glass spring packing to rectify the distilled liquid obtained from S1, and collect the fraction at 33 degrees. In this temperature range, the isomers begin to evaporate and di...

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Abstract

The invention discloses a synthesis method of 3-methyl-2-butyl mercaptan, which comprises the following steps: dehydrating tert-amyl alcohol to obtain trimethyl ethylene, reacting the trimethyl ethylene with thioacetic acid to obtain ethyl thioacetate, stirring at room temperature, hydrolyzing the ethyl thioacetate, and introducing nitrogen for protection to obtain the 3-methyl-2-butyl mercaptan; the extraction process comprises the following steps: S1) mixing and dehydrating; s2) distilling and separating out; s3) reacting to prepare ester; s4) performing gas chromatographic analysis and purification; and s5), preparing the 3-methyl-2-butyl mercaptan. According to the synthesis method of 3-methyl-2-butyl mercaptan, the yield of the product is effectively improved, the reaction is carried out at room temperature, the reaction temperature is reduced, the reaction environment is optimized, in the reaction for preparing the 3-methyl-2-butyl mercaptan, a methanol or ethanol solution containing sodium methoxide or sodium ethoxide alkali is adopted, nitrogen is introduced for protection, oxidation side reactions in a traditional preparation process are effectively avoided, and the production rate of the product is increased.

Description

technical field [0001] The invention relates to the technical field of flavors and fragrances, in particular to a method for synthesizing 3-methyl-2-butanethiol. Background technique [0002] As a class of important organic synthesis reagents, mercaptans are often used in the fields of biology, medicine, pesticides, spices and so on. The thiotal / ketonization reaction of thiols with carbonyl compounds is a common method for protecting functional groups, and it is important and widely used in multi-step synthesis or synthesis of natural products. 3-Methyl-2-butanethiol is a A kind of meat-flavored spice with elegant aroma and good natural feeling. It is widely used in the configuration of flavors and fragrances. In the current extraction process, the reaction temperature is too high, and oxidation side reactions are prone to occur during hydrolysis, and the extraction rate is low. Contents of the invention [0003] The technical problem to be solved in the present invention...

Claims

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Application Information

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IPC IPC(8): C07C319/02C07C321/04C07C327/22C07C1/24C07C11/10
CPCC07C319/02C07C327/22C07C1/24C07C2527/054C07C11/10C07C321/04
Inventor 宣富兴邢晓东韩太安
Owner 河南蔚源生物科技有限公司
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