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Method for Synthesizing Cyclopropaneformic Acid Ester in Low Alcohol Solubility Solvent

A cyclopropane ester and solubility technology, which is applied in the separation/purification of carboxylate, preparation of carboxylate, chemical instruments and methods, etc., can solve the problems of large amount of solvent, large demand for solvent, and difficulty in recycling , to achieve the effect of direct continuous feeding, saving solvent consumption, and convenient recycling

Inactive Publication Date: 2019-06-21
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In the azeotropic composition of aromatic hydrocarbons such as toluene and xylene and alcohol, the content of alcohol is relatively low, and because alcohol and aromatic hydrocarbons are miscible, the azeotrope will not be separated after condensation, resulting in low efficiency of solvent azeotropic band sodium methoxide and evaporation. Methanol takes a long time, requires a large amount of solvent, and is difficult to recycle.
Therefore, aromatic hydrocarbon solvents are not very suitable as solvents for the cyclization reaction, and there are problems such as increased generation of by-products, long time for distilling methanol, large amount of solvent, and difficulty in recycling.
[0007] Although the patent CN1125715A provides a solvent-free process for synthesizing methyl cyclopropanate, the process still has problems such as high content of by-products and long time for distilling methanol

Method used

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  • Method for Synthesizing Cyclopropaneformic Acid Ester in Low Alcohol Solubility Solvent
  • Method for Synthesizing Cyclopropaneformic Acid Ester in Low Alcohol Solubility Solvent
  • Method for Synthesizing Cyclopropaneformic Acid Ester in Low Alcohol Solubility Solvent

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Embodiment 1

[0042] Embodiment 1, a kind of synthetic method of cyclopropyl carboxylate, carries out following steps successively:

[0043] (1), add 68.3g (0.5mol) of methyl 4-chlorobutyrate to a 250mL four-neck flask equipped with a thermometer, a stirring paddle, a dropping funnel, and a 10cm rectification column with a condensing reflux device on the top, and 75 g of alkane, after heating up to 125° C., began to drop (dropping time: 120 min) sodium methoxide methanol solution (containing 0.51 mol of sodium methoxide) with a mass concentration of 30%. Methanol and n-octane are distilled out azeotropically, and the azeotrope is condensed and separated into phases, and the methanol phase in the lower layer is continuously separated.

[0044] When no methanol phase separates out of the n-octane-sodium methylate azeotropic condensate, the cyclization reaction ends, and the cyclization reaction liquid is obtained.

[0045] (2), 82 g of the separated methanol phase was washed with 10 g of wat...

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Abstract

The invention discloses a method for synthesizing cyclopropanecarboxylate by using a low-alcohol solubility solvent. The method comprises the following steps: 1, mixing gamma-chlorobutyrate with a solvent to obtain a mixed base material, heating the obtained mixed base material to 120-130 DEG C, continuously dropwise adding a corresponding alcohol solution of sodium alkoxide or potassium alkoxide to the 120-130 DEG C mixed base material, distilling off solvent-alcohol azeotrope in an azeotropic distillation manner, condensing the obtained azeotrope to layer the azeotrope, and separating the obtained alcohol phase which is a lower condensate layer, and obtaining a cyclization reaction solution after the cyclization reaction ends when no alcohol phase is separated from the azeotropic condensate, wherein the solvent is the low-alcohol solubility solvent; 2, washing the separated alcohol phase obtained in step 1 with water, and separating the obtained organic layer positioned at an upper layer; and 3, mixing the cyclization reaction solution obtained in step 1 with the organic phase obtained in step 2, and carrying out normal pressure rectification to obtain the cyclopropanecarboxylate.

Description

technical field [0001] The invention relates to a synthesis method of cyclopropanecarboxylate, especially a synthesis method using gamma-chlorobutyrate as a starting material. Background technique [0002] Cyclopropyl carboxylate (s-1) is an important intermediate for the synthesis of cyclopropylamine, and cyclopropylamine is an important intermediate for quinolone antibacterial agents, insecticides, and pesticides. [0003] [0004] At present, in the synthetic method of cyclopropanate, most are starting raw material with γ-chlorobutyrate, utilize sodium alkoxide or potassium alkoxide as the strong base of cyclization reaction, aromatic hydrocarbon solvents such as toluene, xylene are solvents, Carry out ring closure reaction at 60~130°C to prepare cyclopropanecarboxylate. [0005] Patent US3711549 utilizes solid sodium methoxide as a strong base and toluene as a solvent to synthesize methyl cyclopropanate by dropping methyl gamma-chlorobutyrate into a sodium methoxide-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/317C07C69/74
CPCC07C67/317C07C67/48C07C67/54C07C69/74
Inventor 陈新志张恒钱超
Owner ZHEJIANG UNIV
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