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Method for preparing hydrosulfuryl acetate using phase transfer catalytic method

A phase transfer catalysis method and thioglycolic acid ester technology are applied in the preparation of mercaptans, organic chemistry and other directions, which can solve the problems of difficult reaction, limited types, and high cost, and achieve simple and easy process, easy availability of raw materials, and applicable aspects. wide effect

Inactive Publication Date: 2006-07-26
康富春
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage of this method is that the cost is too high, the price of thioglycolic acid is too expensive and the types of esters are limited, because lower alcohols and water are miscible and cannot carry water, and higher alcohols and polyols have too high boiling points and cannot carry water; secondary alcohol esters, tertiary alcohol esters And phenolic ester reaction is not easy to carry out, the productive rate is too low and has no industrial value, so this method is limited to a few kinds of esters

Method used

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  • Method for preparing hydrosulfuryl acetate using phase transfer catalytic method

Examples

Experimental program
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Effect test

Embodiment 1

[0020] In a 500ml three-necked flask equipped with mechanical stirring, a thermometer, and a dropping funnel, add 80g (1.0mol) of 70% solid sodium hydrosulfide (industrial product, the same below), 32g of deionized water and 1g of triethylbenzyl ammonium chloride , cooled to 5°C, added 121g (0.9mol) propenyl chloroacetate dropwise under vigorous stirring, and continued to react for 2 hours after dropping, the internal temperature did not exceed 15°C; the lower layer was separated, and the upper layer was washed with deionized water until neutral. Distilled under reduced pressure to obtain 108 g of a colorless transparent liquid with a yield of 91%.

[0021] Elemental analysis (%): C: 45.8 (45.5); H: 6.12 (6.06); O: 24.1 (24.2).

[0022] Note: The theoretical values ​​in brackets are the same below.

Embodiment 2

[0024] The device is the same as in Example 1, add 187g (1.0mol) of 30% industrial sodium hydrosulfide solution and 1.5g of cetyltrimethylammonium bromide, cool to 10°C, and add dropwise 175g (0.85mol) of chlorine under vigorous stirring 2-Ethylhexyl acetate, continue to stir for 5 hours after dripping, the internal temperature does not exceed 20 ° C, the post-treatment method is the same as that of Example 1, and 163 g of a colorless transparent liquid is obtained, and the yield is 94%.

[0025] Elemental analysis (%): C: 58.4 (58.8); H: 10.12 (9.8); O: 15.9 (15.7).

Embodiment 3

[0027] The device is the same as in Example 1, add 80g (1.0mol) of 70% sodium hydrosulfide, 32g of deionized water and 1.2g of tetrabutylammonium bisulfate, and drop 159g (0.9mol) of chloroacetic acid at room temperature (20-25°C) Cyclohexyl ester was stirred and reacted for 5 hours after the dripping was completed, and the internal temperature was not more than 30° C., left to stand, and the post-treatment method was the same as in Example 1 to obtain 150.3 g of a colorless transparent liquid with a yield of 96%.

[0028] Elemental analysis (%): C: 55.3 (55.2); H: 8.14 (8.05); O: 18.2 (18.4).

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Abstract

The invention discloses a preparation method for thioglycollate ester by phase-transfer catalysis, which comprises: (1) dripping ethyl chloroacetate into the mixed liquid of NaHS, H2O and phase-transfer catalyst at room temperature, vigorous stirring and reacting for 1~12h; (2) keeping static for lamination; separating the lower water; cleaning the upper ester with water to neutrality; reducing pressure to distill and obtain the final product. This invention has high yield with low cost.

Description

technical field [0001] The invention relates to a preparation method of thioglycolate, in particular to a method for preparing thioglycolate by a phase-transfer catalytic method. Background technique [0002] Thioglycollate is an important class of fine chemicals, widely used in industrial production. Such as molecular weight regulator in polymer polymerization, PVC organotin heat stabilizer, polythioglycolate (such as trimethylol propane trimercaptoacetate, pentaerythritol tetramercaptoacetate) can also be used as epoxy resin for low-temperature curing Agents, adhesives and optical lenses, etc., with the continuous expansion of its application, the production scale of thioglycolate is also increasing. [0003] There are currently two methods for the preparation of thioglycolic acid esters: the first method is to react with thioglycolic acid and excess alcohol, and use excess alcohol to carry water to promote the reaction. For example the method of CN9010816.2. The disadv...

Claims

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Application Information

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IPC IPC(8): C07C319/02C07C321/04
Inventor 康富春
Owner 康富春
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