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

Method used

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

Examples

Experimental program
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Example Embodiment

[0018] Example 1

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

[0020] 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 5 minutes; turn on the heating device and raise the temperature to 130°C;

[0021] Step 3) Turn on the metering pump, and pump diethylene glycol, 3,5-dichloro-2-pentanone and potassium fluoride into the tubular reactor at a molar ratio of 3:1:1, and check at the outlet The content of 3,5-dichloro-2-pentanone is less than or equal to 0.5%; the mixed liquid directly enters the thin film evaporator, the temperature of the evaporator is controlled at 100℃, the vacuum degree is 500Pa, and 126kg of 1-acetyl-1-chlorocyclopropane is collected on the top. The yield is 98%, and the content is 96%.

Example Embodiment

[0022] Example 2

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

[0024] 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 1 min; turn on the heating device and increase the temperature to 150°C;

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

Example Embodiment

[0026] Example 3

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

[0028] Step 2) Add 82kg of anhydrous sodium 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 9 minutes; turn on the heating device and increase the temperature to 120°C;

[0029] Step 3) Turn on the metering pump, and pump triethylene glycol, 3,5-dichloro-2-pentanone and alkali into the tubular reactor at a molar ratio of 5:1:2, and check at the outlet 3. The content of 5-dichloro-2-pentanone is less than or equal to 0.5%; the mixed liquid directly enters the thin film evaporator, the temperature of the evaporator is controlled at 100℃, the vacuum degree is 200Pa, and the top 1-acetyl-1-chlorocyclopropane 105kg 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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