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Continuous preparation method of 1-acetyl-1-chlorocyclopropane

A technology of chlorocyclopropane and acetyl, which is applied in the field of continuous preparation of 1-acetyl-1-chlorocyclopropane, can solve the problems of long contact time, low production efficiency, and reduced yield, so as to prevent decomposition and deterioration and improve production Efficiency, the effect of simplifying the difficulty of operation

Inactive Publication Date: 2015-06-03
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the post-treatment process of this method, once the 1-acetyl-1-chlorocyclopropane produced in the reaction process cannot be separated from the alkaline reaction solution rapidly, it will contact with the alkali for too long, and it will easily deteriorate and reduce the yield.
Therefore, the technical operation of this process is complicated, and it is not suitable for industrialized production. The yield is generally about 50%, and the production efficiency is low.

Method used

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  • Continuous preparation method of 1-acetyl-1-chlorocyclopropane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Step 1) Add 318kg of diethylene glycol and 155kg of 3,5-dichloro-2-pentanone into the preheated reaction kettle respectively, and heat up to 80°C;

[0020] Step 2) Add 58 kg of anhydrous potassium fluoride to the solid feed port; start the agitator of the tubular reactor, adjust the speed to control the material to stay in the reactor for 5 minutes; turn on the heating device and raise the temperature to 130 ° C;

[0021] Step 3) Turn on the metering pump, inject diethylene glycol, 3,5-dichloro-2-pentanone, and potassium fluoride into the tubular reactor in a molar ratio of 3:1:1, and detect at the outlet The content of 3,5-dichloro-2-pentanone≤0.5%; the mixed solution directly enters the thin-film evaporator, the temperature of the evaporator is controlled at 100°C, the vacuum degree is 500Pa, and 126kg of 1-acetyl-1-chlorocyclopropane at the top is collected, Yield 98%, content 96%.

Embodiment 2

[0023] Step 1) Add 318kg of diethylene glycol and 155kg of 3,5-dichloro-2-pentanone into the preheated reaction kettle respectively, and heat up to 50°C;

[0024] Step 2) Add 58kg of anhydrous potassium fluoride to the solid feed port; start the agitator of the tubular reactor, adjust the speed to control the material to stay in the reactor for 1min; turn on the heating device and raise the temperature to 150°C;

[0025] Step 3) Turn on the metering pump, inject diethylene glycol, 3,5-dichloro-2-pentanone, and potassium fluoride into the tubular reactor in a molar ratio of 3:1:1, and detect at the outlet The content of 3,5-dichloro-2-pentanone is ≤0.5%; the mixed liquid enters the thin-film evaporator directly, the temperature of the evaporator is controlled at 80°C, the vacuum degree is 200Pa, and 119kg of 1-acetyl-1-chlorocyclopropane is collected at the top, Yield 93%, content 95%.

Embodiment 3

[0027] Step 1) Add 750kg of triethylene glycol and 155kg of 3,5-dichloro-2-pentanone into the preheated reaction kettle respectively, and heat up to 50°C;

[0028] Step 2) Add 82 kg of anhydrous sodium fluoride to the solid feeding port; start the agitator of the tubular reactor, adjust the speed to control the material to stay in the reactor for 9 minutes; turn on the heating device and raise the temperature to 120 ° C;

[0029] Step 3) Turn on the metering pump, inject triethylene glycol, 3,5-dichloro-2-pentanone, and alkali into the tubular reactor at a molar ratio of 5:1:2, and detect 3, The content of 5-dichloro-2-pentanone≤0.5%; the mixed solution directly enters the thin-film evaporator, the temperature of the evaporator is controlled at 100°C, the vacuum degree is 200Pa, and 105kg of 1-acetyl-1-chlorocyclopropane at the top is collected, and the yield is 82%, content 96%.

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Abstract

The invention discloses a continuous preparation method of 1-acetyl-1-chlorocyclopropane. A tubular reactor is applied to the preparation process of the 1-acetyl-1-chlorocyclopropane, and the tubular reactor, a solid-liquid feeding pump, a film evaporator and matched equipment are adopted. The continuous preparation method is superior to methods in the prior art and comprises steps as follows: 3,5-dichloro-2-pentanone, a solvent and an alkali are fully mixed and react in the tubular reactor, a reaction liquid is transferred out of the tubular reactor timely and transferred into the film evaporator synchronously to be separated, and a qualified product is obtained. The method has the benefits as follows: the retention time of the product in the reaction liquid is short, so that deterioration is avoided; the continuous preparation method of the 1-acetyl-1-chlorocyclopropane is realized, the production efficiency and the yield are high, and the operation is convenient.

Description

technical field [0001] The invention relates to a method for a pesticide intermediate, in particular to a method for continuously preparing 1-acetyl-1-chlorocyclopropane. technical background [0002] Prothioconazole is recognized as one of the most promising triazole fungicides. It has many advantages such as low toxicity, no teratogenicity, no mutagenicity, no toxicity to embryos, and safety to humans and the environment. . 1-acetyl-1-chlorocyclopropane is an important intermediate required in the synthesis of prothioconazole (US4913727; US6201128). It is usually obtained by removing a molecule of hydrogen chloride from 3,5-dichloro-2-pentanone. In the prior art (US2005 / 222451), 3,5-dichloro-2-pentanone adopts a kettle reaction method, under the action of a phase transfer catalyst, reacts with a base, mixes rapidly, reacts for 2-10min, and quenches Reaction, the product is obtained after post-processing. However, in the post-treatment process of this method, once the 1...

Claims

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Application Information

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IPC IPC(8): C07C49/327C07C45/65
CPCC07C45/65C07C45/82C07C2601/02
Inventor 张晓光宁斌科李秉擘林双政毛明珍徐泽刚杨翠凤张媛媛张建功黄晓瑛何琦文
Owner XIAN MODERN CHEM RES INST
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