Method for producing mercaptoacetic acid ethyl ester

A technology of ethyl mercaptoacetate and ethyl acetate, applied in the field of organic chemical synthesis, can solve the problems of complicated process and high cost, and achieve the effects of simple process, improved yield and short synthesis route

Inactive Publication Date: 2008-06-11
NORTHWEST NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this method is that cost is too high, because lower alcohol and water miscibility cannot carry water, and higher alcohol and polyalcohol boiling point are too high and cannot carry water; The second method is to react (referring to CN1058393A) with specific alcohol with chloroacetic acid, After this method prepares isooctyl chloroacetate, react with sodium thiosulfate to form a salt, and then hydrolyze and reduce.

Method used

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  • Method for producing mercaptoacetic acid ethyl ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Embodiment 1: in the round bottom flask of 100ml, add the mercaptoacetic acid of 27.6g (300mmol), the ethanol of 20.7g (450mmol), the cyclohexane of 16ml, the magnesium perchlorate of 3.34g (15mmol), under stirring Heat to reflux, water will continue to come out from the water separator, stop the reaction until no more water is separated out; distill off excess alcohol and cyclohexane under normal pressure, then add 10ml of distilled water, and then extract with diethyl ether (10ml×3) , organic phase with MgSO 4 Dry, filter, remove ether, then distill under reduced pressure at 80-82°C / 1.3KPa-1.35KPa, collect fractions to obtain ethyl thioglycolate with a yield of 90%. The characterization data of gained ethyl thioglycolate product are as follows:

[0016] IR (KBr): 3433, 2922, 2854, 1740, 1596, 1461, 1423, 1251, 1118, 1040, 801, 671, 621.

[0017] 1 HNMR (400MHz, CDCl 3 , δppm): 4.23-4.17 (m, 2H), 3.26-3.22 (m, 2H), 2.02-1.98 (m, 1H), 1.31-1.23 (m, 3H).

[0018] 1...

Embodiment 2

[0019] Embodiment 2: in the round bottom flask of 100ml, add the mercaptoacetic acid of 27.6g (300mmol), the ethanol of 27.6g (600mmol), the cyclohexane of 16ml, the magnesium perchlorate of 3.34g (15mmol), under stirring Heat to reflux, water will continue to come out from the water separator, stop the reaction when no more water is separated, distill off excess alcohol and cyclohexane under normal pressure, then add 10ml of distilled water, and then extract with diethyl ether (10ml×3) , organic phase with MgSO 4 Dry, filter, remove ether, then distill under reduced pressure at 80-82°C / 1.3KPa-1.35KPa, collect fractions to obtain ethyl thioglycolate with a yield of 90%. The characterization data of the obtained ethyl thioglycolate product are the same as in Example 1.

Embodiment 3

[0020] Embodiment 3: in the round bottom flask of 100ml, add the mercaptoacetic acid of 27.6g (300mmol), the ethanol of 27.6g (600mmol), the cyclohexane of 16ml, the magnesium perchlorate of 6.69g (30mmol), under stirring Heat to reflux, water will continue to come out from the water separator, stop the reaction when no more water is separated, distill off excess alcohol and cyclohexane under normal pressure, then add 10ml of distilled water, and then extract with diethyl ether (10ml×3) , organic phase with MgSO 4 Dry, filter, remove ether, then distill under reduced pressure at 80-82°C / 1.3KPa-1.35KPa and collect fractions to obtain ethyl thioglycolate with a yield of 98%. The characterization data of the obtained ethyl thioglycolate product are the same as in Example 1.

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Abstract

The invention discloses a preparation method of ethyl petrol thioglycolate, which uses magnesium perchlorate as catalyst, uses cyclohexane as water-carrying agent, reacts mercaptoacetic acid with over absolute ethyl alcohol, distills the reaction solution at normal pressure to obtain over alcohol and cyclohexane, washes via distilled water, extracts via ether to remove magnesium perchlorate, filters and dries, depressurizes and distills to obtain ethyl petrol thioglycolate. The invention has simple process, non pollution, low cost and high yield as 98%.

Description

technical field [0001] The invention belongs to the field of organic chemical synthesis, and relates to a method for preparing organic chemical raw material mercaptocarboxylate, in particular to a method for preparing ethyl thioglycolate. 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, can also be used as plasticizer and polysilane lubricant additive, which is beneficial to improve its load performance. Polymercaptoacetate (such as trimethylolpropane trimercaptoacetate, pentaerythritol tetramercaptoacetate) can also be used as a low-temperature curing agent for epoxy resins, making adhesives and optical lenses, etc. With the continuous development of the application of thioglycolate, the production scale of thioglycolate is also increasing. [0003] The preparation of thioglycolic acid ester, existing two k...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/52C07C319/12
Inventor 胡雨来李贵花徐长明牛腾王海峰黄丹凤
Owner NORTHWEST NORMAL UNIVERSITY
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