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Process method for synthesizing and purifying 4-chlorobutyryl chloride

A technology of chlorobutyryl chloride and a process method, applied in the directions of acid halide preparation, chemical recovery, etc., can solve problems such as inability to guarantee product purity, difficult disposal of organic matter, pollution of surrounding environment, etc. good stability

Inactive Publication Date: 2015-05-06
HUBEI BIOCHEM PHARMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The yield of this method can reach more than 90%, the conditions are mild, and it is suitable for industrial production. However, most of the organic solvents used are toxic substances, and the by-products produced are many, so the purity of the products cannot be guaranteed. Pollution

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 1. Preparation of Mixed Catalyst

[0024] Mix 21.3kg of ZnO and 4.2Kg of CuO, add 44.3Kg of 98% concentrated sulfuric acid to react, cool the resulting reactant and dry it at 350°C to obtain the product;

[0025] 2. Add 1000kg of γ-butyrolactone and 50kg of newly prepared mixed catalyst to the reactor, stir, and at the same time, enter tap water into the jacket of the reactor to cool; slowly add 2000kg of thionyl chloride into the reactor from the elevated tank, and add After the completion, the hot water in the jacket was slowly heated to 50-80°C, kept for 5-7 hours for acylation reaction, and the excess thionyl chloride was recovered by negative pressure distillation. The liquid is ready for use; the catalyst in the lower layer can be recycled;

[0026] 3. Pump the supernatant liquid into the crude distillation still and distill under reduced pressure at -0.095MPa~-0.1MPa, accept the fractions in sections, and the fractions before 50°C are mainly thionyl chloride and...

Embodiment 2

[0030] 1. Mix 30.7kg ZnO and 7.5Kg CuO, add 60Kg 98% concentrated sulfuric acid to react, cool the obtained reactant and dry it at 400°C to obtain it;

[0031] 2. Add 1000kg of γ-butyrolactone and 70kg of newly prepared mixed catalyst to the reactor, stir, and at the same time enter tap water into the jacket of the reactor to cool; slowly add 2500kg of thionyl chloride into the reactor from the elevated tank, and add After the completion, the hot water in the jacket was slowly heated to 50-80°C, kept for 5-7 hours to carry out the acylation reaction, the excess thionyl chloride was recovered by negative pressure distillation, and the precipitation was carried out for 8-10 hours after cooling down to normal temperature, and the supernatant was taken The liquid is ready for use; the catalyst in the lower layer can be recycled;

[0032] 3. Pump the supernatant liquid into the crude distillation still and distill under reduced pressure at -0.095MPa~-0.1MPa, accept the fractions i...

Embodiment 3

[0036] 1. Mix 14.4kg ZnO and 4.7Kg CuO, add 37.9Kg 98% concentrated sulfuric acid for reaction, cool the obtained reactant and dry it at 320°C to obtain it;

[0037] 2. Add 1000kg of γ-butyrolactone and 30kg of mixed catalyst to the reactor, stir, and at the same time enter the tap water into the jacket of the reactor to cool; slowly add 1500kg of thionyl chloride into the reactor from the head tank, after the addition is completed Enter the hot water in the jacket and slowly raise the temperature to 50-80°C, keep it warm for 5-7 hours to carry out the acylation reaction, and recover the excess thionyl chloride by negative pressure distillation. After cooling down to normal temperature, it will precipitate for 8-10 hours. use; the lower catalyst can be recycled;

[0038] 3. Pump the supernatant liquid into the crude distillation still and distill under reduced pressure at -0.095MPa~-0.1MPa, accept the fractions in sections, and the fractions before 50°C are mainly thionyl chl...

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Abstract

The invention discloses a process method for synthesizing and purifying 4-chlorobutyryl chloride. The process method comprises the following steps of reacting gamma-butyrolactone and thionyl chloride in the presence of a mixed catalyst to synthesize a 4-chlorobutyryl chloride crude product and purifying the 4-chlorobutyryl chloride crude product to obtain the 4-chlorobutyryl chloride finished product of which the purity is equal to or greater than 99%, the individual impurity is less than 0.30% and the yield is equal to or greater than 90%. In the process method, exhaust gas generated in the production of 4-chlorobutyryl chloride is comprehensively utilized to produce a 30% hydrochloric acid and sodium sulfite solution and the tail material is used for producing 4-chlorobutyric acid ester. The process method is simple, convenient to operate, high in yield and purity of a product and almost free of emission of three wastes and is environmentally friendly.

Description

technical field [0001] The invention relates to a process for synthesizing and purifying 4-chlorobutyryl chloride. Background technique [0002] 4-Chlorobutyryl chloride is an important organic synthesis, pesticide and pharmaceutical intermediate. In the pesticide industry, it can be used to prepare insecticides such as fenthrin and other plant protection agents, and it is also an important intermediate of glufosinate-ammonium. In the pharmaceutical industry, 4-chlorobutyryl chloride is used in the production of antipsychotic drugs trihaloperidol, trifluoropiperidine benzene, quinolone antibacterial drugs ciprofloxacin, ciprofloxacin, sparfloxacin, etc. and antiepileptic drugs Drugs such as levetiracetam. [0003] The existing industrialized production method of 4-chlorobutyryl chloride is mainly obtained by chlorination of gamma-butyrolactone and thionyl chloride under the catalysis of zinc chloride, the yield is about 82%, and the process operation is simple, but gamma ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/58C07C53/50
CPCY02P20/584C07C51/58
Inventor 邹远龙张闻艺陈仁
Owner HUBEI BIOCHEM PHARMA TECH
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