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Method for preparing 3-chloro-2,2-dimethylpropionyl chloride

A technology of dimethylpropionyl chloride and dimethylpropionic acid, which is applied in the field of preparation of 3-chloro-2,2-dimethylpropionyl chloride, can solve the problems of harsh reaction conditions and long reaction time, and achieve mild conditions. Easy to control, low cost, high yield

Inactive Publication Date: 2018-10-23
JIANGSU LIANHE CHEM TECH +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The problem to be solved by the present invention is the defects such as harsh reaction conditions and long reaction time in the preparation method of existing 3-chloro-2,2-dimethylpropionyl chloride. Therefore, the present invention provides a method different from the prior art The preparation method of 3-chloro-2,2-dimethylpropionyl chloride has the advantages of simple process, easy operation, mild condition and easy control, low energy consumption, low cost, high yield, high purity, cleaner reaction, and no Pollution, by-product hydrochloric acid can be comprehensively utilized, suitable for industrial production

Method used

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  • Method for preparing 3-chloro-2,2-dimethylpropionyl chloride

Examples

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Effect test

Embodiment 1

[0032] Add 200g of 3-chloro-2,2-dimethylpropionic acid into the reaction kettle, raise the temperature to 50°C, heat it for 0.5h after melting, add 10g of DMF, continue to keep it for 0.5h, in the range of 50-60°C, feed 150g of phosgene gas, 2.0h ventilation is completed, then maintain the temperature of the kettle at 50-60°C, degas under reduced pressure (vacuum degree of 100mbar) for 2h, and finally obtain 222.93g of 3-chloro-2,2-dimethylpropionyl chloride, the yield 98.2%, gas chromatography detection product purity A% is 98.7%. That 1 H NMR (CDCl 3 ): δ3.61(s, 2H), δ1.39(s, 6H); IR(KBr) main absorption peaks are 2987, 2942, 1811, 1791, 1471, 1391, 923, 880, 811cm -1 ; 1 Both H NMR and IR agree well with the standard spectra.

Embodiment 2

[0034] Add 200g of 3-chloro-2,2-dimethylpropionic acid into the reaction kettle, raise the temperature to 70°C, heat it for 0.5h after melting, add 20g of DMF, continue to keep it for 0.5h, in the range of 70-80°C, feed 148g of phosgene gas, 3.0h ventilation is completed, then maintain the temperature of the kettle at 70-80°C, degas under reduced pressure (vacuum degree 100mbar) for 0.5h, and finally obtain 221.57g of 3-chloro-2,2-dimethylpropionyl chloride, The yield was 97.6%, and the product purity A% detected by gas chromatography was 98.2%. Identification data is with embodiment 1, 1 Both H NMR and IR agree well with the standard spectra.

Embodiment 3

[0036] Add 200g of 3-chloro-2,2-dimethylpropionic acid into the reaction kettle, raise the temperature to 90°C, heat it for 0.5h after melting, add 15g of DMF, keep the heat for 0.5h, in the range of 90-95°C, feed 155g of phosgene gas, 2.0h ventilation is completed, then maintain the temperature of the kettle at 90-95 ° C, degassing under reduced pressure (vacuum degree of 100mbar) for 0.5h, and finally obtain 224.75g of 3-chloro-2,2-dimethylpropionyl chloride, received The yield is 99.0%, and the product purity A% detected by gas chromatography is 98.9%. Identification data is with embodiment 1, 1 Both H NMR and IR agree well with the standard spectra.

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Abstract

The invention discloses a method for preparing 3-chloro-2,2-dimethylpropionyl chloride. The method is characterized in that 3-chloro-2,2-dimethylpropioric acid and phosgene undergo an acylating chlorination reaction in the presence of a catalyst to obtain the 3-chloro-2,2-dimethylpropionyl chloride. The method has the advantages of simple process, easiness in operation, mild and easily-controlledconditions, low energy consumption, low cost, high yield, high purity, clean reaction, no pollution, realization of comprehensive utilization of a byproduct hydrochloric acid, and suitableness for industrial production.

Description

technical field [0001] The invention relates to a preparation method of 3-chloro-2,2-dimethylpropionyl chloride. Background technique [0002] Chloropivaloyl chloride, English name Chloropivaloyl Chloride, alias 3-chloro-2,2-dimethylpropionyl chloride, referred to as CPC, is used as a pharmaceutical and pesticide intermediate, and can be used for the pesticide herbicides clomazone and clomazone Synthesis. It is a colorless irritating liquid at room temperature, with a boiling point of 160°C and a relative density of 1.199. It is soluble in organic solvents such as ethers and toluene. [0003] 3-Chloro-2,2-dimethylpropionyl chloride is widely used in organic synthesis and pesticide intermediates. There are two main methods for its synthesis: one is the reaction of 3-chloro-2,2-dimethylpropionic acid and thionyl chloride to prepare 3-chloro-2,2-dimethylpropionyl chloride. In this process, the protection of inert gas argon is needed, the reaction conditions are harsh, and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/60C07C53/50
CPCC07C51/60C07C53/50
Inventor 王永伟吴斌黄小君
Owner JIANGSU LIANHE CHEM TECH
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