Method for synthesizing 4-chlorobutyryl chloride
A synthesis method and technology of chlorobutyryl chloride are applied in chemical instruments and methods, preparation of acid halides, preparation of organic compounds, etc., can solve problems such as high cost of raw materials, high operation requirements, reduced yield and the like, and achieve high reaction yield , safe operation, mild reaction conditions
Inactive Publication Date: 2018-11-23
杨秀莲
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Problems solved by technology
This method has high yield, the raw material phosgene is cheaper than thionyl chloride, the process is simple, and there is no SO 2 Exhaust gas and three wastes are less, but the chlorinated reagent phosgene itself is a highly toxic chemical, and it is inconvenient to transport and store, and the operation requirements are high
[0006] In CN104086402A, it is proposed to take bis(trichloromethyl)carbonate as chlorination reagent, synthesize 4-chlorobutyryl chloride by gamma-butyrolactone, in the reaction, use organic amine as catalyst, use phase transfer catalyst simultaneously , the yield of this method is high, but post-processing is difficult, the separation cost increases during industrialization, and the yield decreases significantly when it is scaled up to industrial production
[0007] In CN104592001A, it is proposed to use gamma-butyrolactone and thionyl chloride to react under a mixed catalyst, and the resulting product has high purity, but there are still problems of high raw material cost, high toxicity, and more three wastes
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preparation example 1
[0030] According to the intercalation reaction characteristics of aluminum dihydrogen tripolyphosphate and organic amine, the method described in Applied Chemistry, 2014, 31 (7), add methylamine and water in the reactor, dissolve, put aluminum dihydrogen tripolyphosphate , stirred and reacted at room temperature, and separated to obtain catalyst A.
preparation example 2
[0032] According to the same method as catalyst preparation example 1, except adding ethylamine instead of methylamine, the others are the same to obtain catalyst B.
preparation example 3
[0034] According to the same method as catalyst preparation example 1, except adding pyridine instead of methylamine and water, the rest are the same to obtain catalyst C.
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The invention relates to a method for synthesizing 4-chlorobutyryl chloride, which is characterized in that gamma-butyrolactone and di(trichloromethyl) carbonate are used as reaction raw materials, and a specific amine catalyst is used for carrying out chlorination reaction to obtain 4-chlorobutyryl chloride, wherein, the amine catalyst is an intercalation product obtained by reacting aluminum dihydrogen tripolyphosphate with an organic amine, and the structure thereof is as follows: the formulas are shown in the specification, wherein R is an alkyl group and an aromatic group.
Description
technical field [0001] The invention relates to a synthetic method of 4-chlorobutyryl chloride. Background technique [0002] 4-Chlorobutyryl chloride is an important intermediate in organic synthesis, medicine and pesticide. [0003] In the pharmaceutical industry, 4-chlorobutyryl chloride is used in the production of antipsychotic drugs trihaloperidol, tricloperidine benzene, levetiracetam, quinolone antibacterial drugs ciprofloxacin, ciprofloxacin, spar Shaxing et al. In the pesticide industry, it can be used to prepare isoxaflutole, isoxaflutole, etc. [0004] At present, the existing industrial production method of 4-chlorobutyryl chloride is mainly obtained by chlorination of γ-butyrolactone through thionyl chloride under the catalysis of zinc chloride, and the yield is about 82%, but the process is simple to operate , raw materials are easy to get, but the cost of raw materials is relatively high, and there are many three wastes. [0005] In addition, in patents U...
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IPC IPC(8): C07C51/58C07C51/64C07C53/50B01J31/26
CPCB01J31/26C07C51/58C07C51/64C07C53/50
Inventor 杨秀莲
Owner 杨秀莲
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