A method for synthesizing gamma-chlorobutyric acid

A technology of chlorobutyric acid and butyrolactone, applied in the preparation of carboxylate/lactone, organic chemistry, etc., can solve the problems of high operation requirements, potential safety hazards, etc., to avoid high-pressure reaction, avoid danger, and yield high effect

Active Publication Date: 2021-05-07
DAFENG YUELONG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Both of the above two processes require a high-pressure reactor, which requires high operation and poses safety hazards

Method used

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  • A method for synthesizing gamma-chlorobutyric acid
  • A method for synthesizing gamma-chlorobutyric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Put 86 g of γ-butyrolactone into the flask, and keep stirring at room temperature and normal pressure. Add 5g of silicotungstic acid into the flask, keep stirring at room temperature and normal pressure. 200g of 20% hydrochloric acid was slowly added dropwise, and the reaction was stirred for 2h. Sampling and GC analysis showed that the residual gamma-butyrolactone was less than 1%, and the gamma-chlorobutyric acid content reached more than 99%. Leave to stand for stratification, collect the product of the lower layer, and repeat the application of the upper layer of water.

Embodiment 2

[0018] Put 86 g of γ-butyrolactone into the flask, and keep stirring at room temperature and normal pressure. Add 4.3g of phosphotungstic acid into the flask, keep stirring at room temperature and normal pressure. 200g of 20% hydrochloric acid was added dropwise, and the reaction was stirred for 2h. Sampling and GC analysis showed that the residual gamma-butyrolactone was less than 1%, and the gamma-chlorobutyric acid content reached more than 99%. Leave to stand for stratification, collect the product of the lower layer, and repeat the application of the upper layer of water.

Embodiment 3

[0020] The γ-butyrolactone of 86g and the upper strata aqueous phase collected in the example one are put into the flask, keep stirring at room temperature, add 200g of 20% hydrochloric acid dropwise for reaction, after 2h, sample GC analysis, the residue of γ-butyrolactone is less than 1%. The content of γ-chlorobutyric acid reaches more than 99%. Leave to stand for stratification, collect the product of the lower layer, and repeat the application of the upper layer of water. After 10 times of reaction, the content of γ-chlorobutyric acid can still reach more than 90%.

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Abstract

The invention provides a method for synthesizing γ-chlorobutyric acid, which comprises the following steps: putting 86 g of γ-butyrolactone into a flask, stirring at room temperature and normal pressure; adding 1%-10% heteropolyacid catalyst, and stirring at room temperature and normal pressure uniformly; slowly add 200 g of 20% hydrochloric acid dropwise, and stir for 2 hours; after GC detection, the residual γ-butyrolactone is less than 1%, and the content of γ-chlorobutyric acid reaches more than 99%; stand for stratification, and collect the lower product; The upper aqueous phase was applied repeatedly. The present invention selects a catalyst for effective reaction, avoids high-pressure reaction, avoids the danger of using thionyl chloride, and no waste water is generated in the reaction process, the catalyst can be used repeatedly, and the prepared γ-chlorobutyric acid yield is higher.

Description

technical field [0001] The invention belongs to the field of synthesis methods, and more specifically relates to a method for synthesizing gamma-chlorobutyric acid. Background technique [0002] There are two main processes in the prior art: one uses gamma-butyrolactone as raw material, zinc chloride as catalyst, feeds dry hydrogen chloride gas, the reaction temperature is 120°C, the pressure is 2.1MPa, the reaction is stirred for 2 hours and then cooled to obtain γ-chlorobutyric acid; the other uses γ-butyrolactone as a raw material and thionyl chloride as a catalyst to generate γ-chlorobutyryl chloride, which is acidified to obtain γ-chlorobutyric acid. Both of the above two processes require high-pressure reactors, which require high operating requirements and pose potential safety hazards. In the second process, thionyl chloride is used as a catalyst, which is highly corrosive and irritating, and decomposes into sulfur dioxide and hydrogen chloride gas when it encounter...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C53/19C07C51/09
CPCC07C51/09C07C53/19
Inventor 杨采风江以桦
Owner DAFENG YUELONG CHEM
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