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Preparation method of high-purity cyclopropyl methyl ketone

A cyclopropyl methyl ketone, high-purity technology, applied in the field of preparation of cyclopropyl methyl ketone, can solve the problems of high complexity of devices and methods, achieve the effect of solving difficult separation and improving the separation efficiency of rectification

Pending Publication Date: 2021-11-02
JIANGSU QINGQUAN CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method adopts the combination method of rectification and extraction to purify cyclopropyl methyl ketone, and the corresponding devices and methods become highly complicated.

Method used

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  • Preparation method of high-purity cyclopropyl methyl ketone
  • Preparation method of high-purity cyclopropyl methyl ketone
  • Preparation method of high-purity cyclopropyl methyl ketone

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Cyclopropyl methyl ketone reaction solution 1000g, dibenzoyl peroxide 0.5g, stir and heat up to 40°C for 12h, then transfer to rectification kettle, heat up, when the gas phase temperature is 80-90°C, reflux to separate water , after no water is separated out, take out the previous fraction, the gas phase temperature is 114°C, the reflux ratio is 4:1-2:1, sampling and testing, the gas phase content is ≥99.9%, the reflux ratio is 1:1, and the product is received, no fraction is evaporated Go out, stop rectifying, obtain product 924g.

Embodiment 2

[0030] Cyclopropyl methyl ketone reaction solution 1000g, azobisisobutyronitrile 1.0g, stir and heat up to 60°C for 8 hours, then transfer to a rectification kettle, heat up, when the gas phase temperature is 80-90°C, reflux to separate water , after no water is separated out, take out the previous fraction, the gas phase temperature is 114°C, the reflux ratio is 4:1-2:1, sampling and testing, the gas phase content is ≥99.9%, the reflux ratio is 1:1, and the product is received, no fraction is evaporated Go out, stop rectifying, obtain product 947g.

Embodiment 3

[0032] Cyclopropyl methyl ketone reaction solution 1000g, dibenzoyl peroxide 0.5g, stir and heat up to 40°C for 12h, then transfer to rectification kettle, heat up, when the gas phase temperature is 80-90°C, reflux to separate water , after no water is separated out, take out the previous fraction, the gas phase temperature is 114°C, the reflux ratio is 4:1-2:1, sampling and testing, the gas phase content is ≥99.9%, the reflux ratio is 1:1, and the product is received, no fraction is evaporated Go out, stop rectifying, obtain product 915g.

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Abstract

The invention provides a preparation method of high-purity cyclopropyl methyl ketone, which comprises the following steps: carrying out chemical reaction on 5-chloro-2-pentanone to obtain a cyclopropyl methyl ketone reaction solution, and adding a free radical initiator into the cyclopropyl methyl ketone reaction solution to carry out a polymerization reaction on 4, 5-dihydro-2-methyl furan (DHMF) in the cyclopropyl methyl ketone reaction solution to form a 2-methyl furan polymer, so that the cyclopropyl methyl ketone reaction solution becomes a DHMF low-content mixed solution, and carrying out rectification separation on the DHMF low-content mixed solution to obtain a high-purity cyclopropyl methyl ketone product. According to the method, the one-time rectification yield of the product CMPO is greater than 90%, the GC purity of the product CMPO is greater than 99.9%, and the energy consumption is remarkably reduced while the rectification efficiency of the product is improved. Therefore, the invention provides a brand-new and high-efficiency preparation method of high-purity cyclopropyl methyl ketone.

Description

technical field [0001] The invention relates to the field of pharmaceutical intermediates, in particular to a preparation method of cyclopropyl methyl ketone. Background technique [0002] Cyclopropyl methyl ketone (CPMO) is an important intermediate for the synthesis of ciprofloxacin drugs, and also an important intermediate for the synthesis of the anti-AIDS drug efavirenz, the green pesticide cyprodinil and the plant growth regulator cyproconazole body. [0003] [0004] The synthesis of cyclopropyl methyl ketone usually uses 5-chloro-2-pentanone as a raw material to obtain a crude product through cyclization, and then rectifies and separates to obtain a high-purity product. For example, the patent CN200610098154 discloses a preparation method of cyclopropyl methyl ketone, which is to add acetyl n-propanol to hydrochloric acid solution, chlorination reaction occurs, and adopt separation and coupling technology to distill 5-chloro-2-pentanone Out; 5-chloro-2-pentanone...

Claims

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Application Information

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IPC IPC(8): C07C45/65C07C45/78C07C45/85C07C45/82C07C49/293
CPCC07C45/65C07C45/78C07C45/85C07C45/82C07C2601/02C07C49/293
Inventor 徐晓秋刘长乐陈昞志王长锦李亚峰童德兵
Owner JIANGSU QINGQUAN CHEM CO LTD