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Preparation method of 2-chloro-1-(1-chlorocyclopropyl) acetone

A technology of chlorocyclopropyl and ethyl ketone, which is applied in the field of preparation of 2-chloro-1-ethanone, can solve the problems of long reaction route, long reaction cycle, and low reaction yield, and achieve short reaction route and short reaction cycle. Short, easy-to-use effects

Inactive Publication Date: 2019-05-14
HEBEI CHENGXIN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Aiming at the problems of long reaction route, long reaction cycle and complicated operation in the prior art; low reaction yield and low product content, the invention provides a kind of 2-chloro-1-(1-chlorocyclopropyl)ethanone preparation method

Method used

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  • Preparation method of 2-chloro-1-(1-chlorocyclopropyl) acetone

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Embodiment 1

[0030] A preparation method of 2-chloro-1-(1-chlorocyclopropyl)ethanone, comprising the following steps:

[0031] (1) Add 365.0 g (0.5 mol) of hydrochloric acid with a mass concentration of 5% to a 500 ml four-neck flask equipped with a mechanical stirrer, a thermometer, and a reflux water separator, start stirring, and add α-acetyl-γ-butane dropwise Ester 65.0g (0.5mol), heat up and control the reaction temperature to 40-50°C, carry out the ring-opening decarboxylation reaction for 3h, heat up for distillation, distill water and 5-chloro-2-pentanone azeotropically, and reflux the water to The reaction bottle yielded 55.2 g of 5-chloro-2-pentanone, the gas chromatography analysis content was 96.04%, and the molar yield was 90.60%;

[0032] (2) In the 250ml four-necked flask that mechanical stirring, thermometer, normal pressure distillation unit are housed, add the sodium hydroxide solution 133.3g (0.5mol) that mass fraction is 15%, tetrabutyl ammonium bromide 0.3g, open Stir...

Embodiment 2

[0035] A preparation method of 2-chloro-1-(1-chlorocyclopropyl)ethanone, comprising the following steps:

[0036] (1) Add 365.0 g (1.0 mol) of hydrochloric acid with a mass concentration of 10% into a 500 ml four-neck flask equipped with a mechanical stirrer, a thermometer, and a reflux water separator, start stirring, and add α-acetyl-γ-butyl dropwise Lactone 90.0g (0.7mol), heat up and control the reaction temperature at 50-60°C, react for 2.5h, then heat up for distillation treatment to distill water and 5-chloro-2-pentanone azeotropically, and return the water to the reaction flask , to obtain 79.5 g of 5-chloro-2-pentanone, the gas chromatography analysis content was 95.36%, and the molar yield was 89.82%;

[0037] (2) In the 250ml four-neck flask that mechanical stirring, thermometer, atmospheric distillation unit are housed, adding mass concentration is 20% sodium hydroxide solution 150.9g (0.75mol), tetrabutyl ammonium bromide 0.8g, start stirring , quickly drop 79.5g...

Embodiment 3

[0040] A preparation method of 2-chloro-1-(1-chlorocyclopropyl)ethanone, comprising the following steps:

[0041] (1) Add 486.7g (2.0mol) of hydrochloric acid with a mass concentration of 15% to a 1000ml four-neck flask equipped with a mechanical stirrer, a thermometer, and a reflux water separator, start stirring, and add α-acetyl-γ-butyl dropwise Lactone 128.5g (1.0mol), control the reaction temperature at 60-70°C, react for 1.5h, then heat up and carry out distillation treatment to azeotropically distill water and 5-chloro-2-pentanone, and return the water to the reaction bottle to obtain 5 - Chloro-2-pentanone 114.5g, gas chromatography analysis content 96.18%, molar yield 91.34%;

[0042] (2) In the 500ml four-necked flask that mechanical stirring, thermometer, atmospheric distillation unit are housed, adding mass concentration is 205g (1.28mol) of sodium hydroxide solution of 20%, 2.5g of benzyltriethylammonium chloride, open Stir, quickly add 114.5g of 5-chloro-2-penta...

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Abstract

The invention relates to the technical field of chemical synthesis, and particularly discloses a preparation method of 2-chloro-1-(1-chlorocyclopropyl) acetone. The preparation method comprises the following steps: enabling alpha-acetyl-gamma butyrolactone and hydrochloric acid to have an open-loop decarboxylic reaction to obtain 5-chloro-2-pentanone; adding the 5-chloro-2-pentanone and a catalystinto an alkaline solution, implementing a cyclization reaction, obtaining cyclopropyl methyl ketone; implementing a chlorination reaction with a chloride agent to obtain the 2-chloro-1-(1-chlorocyclopropyl) acetone. The reaction steps of the provided method are less, the reaction period is short, the yield is more than 70%, and the content of the 2-chloro-1-(1-chlorocyclopropyl) acetone in a product is more than 95%.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of 2-chloro-1-(1-chlorocyclopropyl)ethanone. Background technique [0002] Prothioconazole (Prothioconazole) is a broad-spectrum, high-efficiency triazolethione fungicide, the chemical name is (RS)-2-[2-(1-chlorocyclopropyl)-3-(2-chloro Phenyl)-2-hydroxypropyl]-2,4-dihydro-1,2,4-triazole-3-thione is mainly used to control many diseases of cereals, wheat and bean crops. The results of a large number of field efficacy tests show that prothioconazole has no environmental risk concerns, good safety for crops, good disease prevention and treatment effects, obvious increase in yield, low toxicity, no teratogenicity, no mutagenicity, and no toxicity to embryos , safe for people and the environment, and is recognized as one of the most promising triazole fungicides. [0003] Prothioconazole and its intermediates have complex structures and are difficult ...

Claims

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Application Information

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IPC IPC(8): C07C45/63C07C49/327
Inventor 张辰亮袁康范李科徐鑫光卢冬梅秦建辉琚朋朋
Owner HEBEI CHENGXIN
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