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Synthetic process of 1-chloro-cyclopropanecarbonyl chloride

A technology for the synthesis of chloroacetylcyclopropane, which is applied in the field of synthesis of 1-chloro-1'-chloroacetylcyclopropane, can solve the problems of low yield and unsuitability for industrial scale-up production, and achieve simple operation, Typical controllable process conditions and effects of smooth process connections

Active Publication Date: 2015-01-21
DALIAN JOIN KING FINE CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The solvents involved in the above process are constantly switched, and the yields of some steps are low, which is obviously not suitable for industrial scale-up production

Method used

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  • Synthetic process of 1-chloro-cyclopropanecarbonyl chloride
  • Synthetic process of 1-chloro-cyclopropanecarbonyl chloride
  • Synthetic process of 1-chloro-cyclopropanecarbonyl chloride

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Synthesis of 1-chloro-1'-chloroacetylcyclopropane.

[0029] (1) Chlorination reaction Ⅰ, synthesis of α-chloro-α’-acetyl-γ-butyrolactone

[0030] Add α-acetyl-γ-butyrolactone 3235.6g (25mol, 99%, 1.0eq) in a 30L jacketed kettle equipped with mechanical stirring, thermometer and tail gas absorption device; cool down to 0°C, start to add sulfuryl chloride dropwise 3408.3g (25mol, 99%, 1.0eq), the temperature control does not exceed 30 ° C, after the dropwise addition is completed, stir for 2 hours until the raw materials are completely converted; after the reaction is completed, remove a small amount of residual sulfuryl chloride, hydrochloric acid gas and sulfur dioxide under reduced pressure to obtain the crude product α -Chloro-α'-acetyl-γ-butyrolactone 4060g yellowish transparent liquid, purity 99.5%, crude yield 100%.

[0031] (2) ring opening reaction, synthesis of 3,5 dichloro-2-pentanone

[0032] Add 4060g α-chloro-α'-acetyl-γ-butyrolactone (25mol, 99.5%, 1.0eq)...

Embodiment 2

[0040] Synthesis of 1-Chloro-1'-Chloroacetylcyclopropane

[0041] The amount of raw materials added in each step and the condition control are the same as in Example 1, and the organic solvent used for extraction in the ring-opening reaction is toluene, so the reaction solvent in other subsequent steps is toluene. The four-step total yield of the product is 101.7%*80%*82%*70%=46.8%.

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Abstract

The invention discloses a synthetic process of 1-chloro-cyclopropanecarbonyl chloride, which belongs to the technical field of fine chemical processes. The process is implemented by taking alpha-acetyl-gamma-butyrolactone and sulfonyl chloride as raw materials through the steps of chlorinating, ring cleavage, cyclization, and re-chlorinating, so that a target product is obtained. The synthetic process is implemented by taking cheap industrial chemicals as raw materials and reaction reagents, and by using a single solvent system, a smooth process connection is achieved, so that the reaction yield is improved, the process operation is simplified, the cost of raw materials is reduced, and the cost of production is lowered.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a synthesis process of 1-chloro-1'-chloroacetylcyclopropane. Background technique [0002] Prothioconazole (prothioconazole), trade name Proline, Input, chemical name (R, S)-2-[2-(1-chlorocyclopropyl)-3-(2-chlorophenyl)-2-hydroxypropyl Base]-2,4-dihydro-1,2,4-triazole-3-thione is a broad-spectrum triazole fungicide developed by Bayer, mainly used to control cereals, wheat and beans crops and many other diseases. Prothioconazole is a racemate, and its pure product is white or light gray-brown powder crystal. Its mechanism of action is to inhibit the demethylation at the 14-position of lanosterol or 2,4-methylene dihydrolanosterol, the precursor of sterol in fungi. Prothioconazole has good biotoxicity and ecotoxicity, and is safe to humans and the environment. Prothioconazole is mainly used to prevent and control diseases of cereal crops such as wheat, barley, rape, pean...

Claims

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Application Information

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IPC IPC(8): C07C49/327C07C45/63
CPCC07C45/59C07C45/61C07C45/63C07C2601/02C07D307/33C07C49/16C07C49/327
Inventor 李雨王海英徐德胜于圣慧李殿虎王荣良
Owner DALIAN JOIN KING FINE CHEM CO LTD
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