CN103193621A - Acylation reaction method for preparing 2-4-(chlorophenyl)-3-methylbutyryl chloride - Google Patents

Abstract

The invention discloses an acylation reaction method for preparing 2-4-(chlorophenyl)-3-methylbutyryl chloride. The acylation reaction method comprises the following steps: adding 900-950 parts by weight of 2-4-(chlorophenyl)-3-methylbutyric acid, 10-12 parts by weight of acetic acid and 20-25 parts by weight of activated carbon into a reaction kettle, dripping 510-520 parts by weight of thionyl chloride into the reaction kettle at normal temperature, performing heat release reaction, increasing the temperature to 80 DEG C, then opening the reaction kettle, stirring, performing heat preservation for 6hours after the end of dripping of the thionyl chloride, and press-filtering out the activated carbon and other impurities to obtain a crude product 2-4-(chlorophenyl)-3-methylbutyryl chloride. According to the acylation reaction method, the activated carbon is adopted for heat absorption, so that the smooth reaction conditions can be ensured, the yield is greatly improved, the acetic acid is increased and the stable reaction conditions are ensured so as to be conductive to performing the reaction.

Description

The acylation reaction method of preparation 2-4-(chloro-phenyl-)-3-Methylbutanoyl chloride

Technical field

It is synthetic to the present invention relates to a kind of compound, specifically is a kind of preparation 2-4-(chloro-phenyl-)-the acylation reaction method of 3-Methylbutanoyl chloride.

Background technology

The 2-4-(chloro-phenyl-)-and 3-Methylbutanoyl chloride is important fine-chemical intermediate, because its purposes constantly is developed and utilizes, the added value of many derived product is all very high in recent years.Domestic research is started late, at present mainly as pesticide intermediate, for the production of fenvalerate, come pyrethroid insectide such as good fortune spirit (intend, be exactly manually copy, the biological pesticide of chemosynthesis).

The 2-4-(chloro-phenyl-)-the 3-Methylbutanoyl chloride productive unit mainly comprises: operations such as alkylation, hydrolysis, neutralization separation, acidifying separation, acidylate.Problems such as existing acylation process exists reaction yield low, and quality is not high.

Summary of the invention

The purpose of this invention is to provide a kind of preparation 2-4-(chloro-phenyl-)-the acylation reaction method of 3-Methylbutanoyl chloride.

Technical scheme of the present invention is as follows:

Preparation 2-4-(chloro-phenyl-)-and the acylation reaction method of 3-Methylbutanoyl chloride, it is characterized in that may further comprise the steps:

2-4-(chloro-phenyl-with the 900-950 weight part)-3 Methylbutanoic acid; the acetic acid of 10-12 weight part; the gac of 20-25 weight part adds in the reactor; the sulfur oxychloride of Dropwise 5 10-520 weight part in the reactor at normal temperatures; reaction is thermopositive reaction; equitemperature rises to 80 ℃; open and stir; after sulfur oxychloride dropwises; be incubated 6 hours; be press-filtered out gac and other impurity; get the 2-4-(chloro-phenyl-)-the 3-Methylbutanoyl chloride crude product; crude product is sucked the still kettle distillation with vacuum pump reclaim excessive sulfur oxychloride; residuum is the 2-4-(chloro-phenyl-at the bottom of the still kettle still)-3-Methylbutanoyl chloride; the HCL that acylation reaction produces; SO2 adopts the falling liquid film secondary to absorb to such an extent that contain the hydrochloric acid soln of sulfurous acid, again with three grades of alkali absorptions.

The present invention adopts the gac heat absorption, can guarantee that reaction conditions is steady, has improved productive rate greatly, increases acetic acid, has guaranteed stable reaction conditions, is conducive to reaction and carries out.

Embodiment

Preparation 2-4-(chloro-phenyl-)-and the acylation reaction method of 3-Methylbutanoyl chloride, may further comprise the steps:

2-4-(chloro-phenyl-with 930 kilograms)-3 Methylbutanoic acid; 10 kilograms acetic acid; 20 kilograms gac adds in the reactor; the sulfur oxychloride of 10 kilograms of Dropwise 5s in the reactor at normal temperatures; reaction is thermopositive reaction; equitemperature rises to 80 ℃; open and stir; after sulfur oxychloride dropwises; be incubated 6 hours; be press-filtered out gac and other impurity; get the 2-4-(chloro-phenyl-)-the 3-Methylbutanoyl chloride crude product; crude product is sucked the still kettle distillation with vacuum pump reclaim excessive sulfur oxychloride; residuum is the 2-4-(chloro-phenyl-at the bottom of the still kettle still)-971 kilograms of 3-Methylbutanoyl chlorides; the HCL that acylation reaction produces; SO2 adopts the falling liquid film secondary to absorb to such an extent that contain the hydrochloric acid soln of sulfurous acid, again with three grades of alkali absorptions.

Claims (1)

1. preparation 2-4-(chloro-phenyl-)-and the acylation reaction method of 3-Methylbutanoyl chloride, it is characterized in that may further comprise the steps:

2-4-(chloro-phenyl-with the 900-950 weight part)-3 Methylbutanoic acid; the acetic acid of 10-12 weight part; the gac of 20-25 weight part adds in the reactor; the sulfur oxychloride of Dropwise 5 10-520 weight part in the reactor at normal temperatures; reaction is thermopositive reaction; equitemperature rises to 80 ℃; open and stir; after sulfur oxychloride dropwises; be incubated 6 hours; be press-filtered out gac and other impurity; get the 2-4-(chloro-phenyl-)-the 3-Methylbutanoyl chloride crude product; crude product is sucked the still kettle distillation with vacuum pump reclaim excessive sulfur oxychloride; residuum is the 2-4-(chloro-phenyl-at the bottom of the still kettle still)-3-Methylbutanoyl chloride; the HCL that acylation reaction produces; SO2 adopts the falling liquid film secondary to absorb to such an extent that contain the hydrochloric acid soln of sulfurous acid, again with three grades of alkali absorptions.