Process for preparing chloro-pivalyl chloride

A technology for chloropivaloyl chloride and crude chloropivaloyl chloride, which is applied in carboxylate preparation, chemical instruments and methods, preparation of organic compounds, etc., can solve problems such as non-industrial production methods, and achieve low cost and easy The effect of control and high yield

Active Publication Date: 2008-11-26
JIANGSU JIANNONG PLANT PROTECTION CO LTD
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Problems solved by technology

Although the above method avoids or partially avoids the existing technical shortcomings of the industrial production process, it is not an ideal industrial production method because of the price of raw materials or the limitation of process conditions.

Method used

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  • Process for preparing chloro-pivalyl chloride
  • Process for preparing chloro-pivalyl chloride

Examples

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Embodiment Construction

[0027] Industrial example: an example of producing 1 ton of chlorpivaloyl chloride with a content above 99.5%.

[0028] 1, in reaction step (1), the pivaloyl chloride (claiming trimethylacetyl chloride again, structural formula is (CH 3 ) 3 CCOCl) molecular formula is C 5 h 9 ClO, molecular weight 120.5)

[0029] Raw materials used (1) pivalic acid, content > 98% (2) phosphorus trichloride, content 98%

[0030] at 2m 3 Drop into 937kg pivalic acid and 405kg phosphorus trichloride in the reactor. Slowly raise the temperature under stirring for 2 hours, rise to 55 ° C, continue to keep warm and stir for 2 hours, let stand to separate the upper layer clear night, rectify, collect the fraction at 104-105 ° C, and obtain 1050 kg of fine pivaloyl chloride, with a content of 99.5%. The rate is above 92%.

[0031] 2. In the reaction step (2), the final product 3-chloro-2,2-dimethylpropionyl chloride (also known as chloropivaloyl chloride, structural formula ClCH 2 (CH 3 ) 2 ...

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Abstract

The invention relates to a preparation method for chloro-pivaloyl chloride, in particular to a method that pivalic acid is taken as starting material to synthesize pivaloyl chloride by phosphorus trichloride acyl chlorination; then, gas-phase photocatalysis chlorination is carried out on the pivaloyl chloride by adopting reactive rectification technique; finally the chloro-pivaloyl chloride is prepared by vacuum rectification. The method of the invention can effectively inhibit the generation of multi chlorine substitutes and has simple production technique, safe operation, no pollution, low production cost and high production quality.

Description

field of invention [0001] The invention relates to a method for preparing chloropivaloyl chloride, specifically, the method uses pivalic acid as a starting material, chlorinates pivaloyl chloride with phosphorus trichloride, and then uses reactive distillation technology to purify pivaloyl chloride. The valeryl chloride is subjected to gas-phase photocatalytic chlorine, and then vacuum distillation is carried out to prepare chloropivaloyl chloride. The invention also relates to a process for the preparation of pivaloyl chloride. Background technique [0002] Chloropivaloyl chloride (also known as 3-chloro-2,2-dimethylpropionyl chloride) is an important acylating reagent and isoxazolone ring-forming reagent, which is widely used in the organic synthesis industry and is currently mainly used as Pharmaceutical intermediates, pesticide intermediates, and as synthetic raw materials for rubber additives and photographic photosensitive materials. [0003] The synthetic precursor ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C53/42C07C51/60
CPCY02P20/10
Inventor 高中良王曙光
Owner JIANGSU JIANNONG PLANT PROTECTION CO LTD
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