Preparation method and preparation device for gamma-chloro-methyl butyrate

Abstract

The invention belongs to the technical field of drug intermediate synthesis, and particularly relates to a preparation method and preparation device for gamma-chloro-methyl butyrate. The preparation method comprises the following steps that gamma-butyrolactone and sulfoxide chloride are fed into a first-level jet mixer to be mixed and then sprayed into a preheater, and the temperature is increased to 30-35 DEG C; the mixture enters a second-level jet mixer, and meanwhile methyl alcohol is added in the second-level jet mixer; after mixing is performed, the mixture is sprayed into a static mixer, and the temperature is controlled at 52-55 DEG C; after a reaction is completed, the temperature is lowered, and then the gamma-chloro-methyl butyrate is obtained. The preparation device comprises the first-level jet mixer, the preheater, the second-level jet mixer, the static mixer and a cooler which are sequentially communicated; the first-level jet mixer and the second-level jet mixer are each provided with two liquid inlets and a liquid outlet, and the static mixer comprises a shell and a temperature control device arranged in the shell. According to the preparation method and preparation device for the gamma-chloro-methyl butyrate, continuous production can be achieved, the production efficiency is high, the product yield is high, and the cost is low.

Description

technical field [0001] The invention belongs to the technical field of synthesis of pharmaceutical intermediates, and in particular relates to a preparation method of methyl γ-chlorobutyrate and a preparation device thereof. Background technique [0002] Cyclopropylamine is an aliphatic amine containing a three-membered ring, which is a very important high value-added drug intermediate, quinolone antibacterial drugs Ciprofloxacin (Ciprofloxacin), Sparfloxacin (Sparfloxacin), Barofloxacin (Balofloxacin) Cyclopropylamine and Tomefloxacin (Tomefloxacin) all use cyclopropylamine as the main intermediate or raw material; in addition, cyclopropylamine is also used in the synthesis of plant protection agents and feed additives. [0003] At present, the production process of cyclopropylamine with industrial value is to use γ-butyrolactone as raw material, undergo ring opening, esterification, and then undergo ring closure and Hoffmann degradation reaction to finally generate cyclopr...

AI Technical Summary

Problems solved by technology

[0005] In industrialized production, the above processes are all completed by batch reactors, which have problems such as high labor intensity and low production efficiency, and manual operation will lead to unstable process conditions and fluctuations in product quality; at the same time, hydrogen chloride, Sulfur dioxide and other waste gas treatment methods are still the traditional way of absorbing hydrogen chloride with water, and then using ammonia water to absorb sulfur dioxide to prepare ammonium bisulfite. Due to unsalable by-products, normal production is affected. At the same time, hydrogen chloride and sulfur dioxide gases leaked during the absorption process are very corrosive and pollute the environment.

[0006] Because the reaction process of gamma-butyrolactone to prepare gamma-chlorobutyric acid methyl ester is a batch process, and the production process needs to be continuously heated, cooled, etc., not only reduces production efficiency, increases energy consumption, but also the hydrogen chloride and The process of sulfur dioxide and other gases cannot be continuously produced, and the method of continuous pressurized rectification cannot be used for subsequent treatment, which also increases the difficulty of efficient resource utilization of waste gas; to change the above problems, this traditional reaction process must be changed

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