Preparation method of benzoyl area kind derivative

A technology for benzoyl urea and derivatives is applied in the field of preparation of benzoyl urea derivatives, which can solve the problems of large potential safety hazard, high production cost, equipment corrosion and the like, and achieves safe and reliable production, low production cost, less corrosive effect

A technology for benzoyl urea and derivatives is applied in the field of preparation of benzoyl urea derivatives, which can solve the problems of large potential safety hazard, high production cost, equipment corrosion and the like, and achieves safe and reliable production, low production cost, less corrosive effect

CN1903838AInactive Publication Date: 2007-01-31ZHEJIANG UNIV OF TECH
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  • Preparation method of benzoyl area kind derivative
  • Preparation method of benzoyl area kind derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] In a 500mL three-necked flask, install a dropping funnel, a reflux condenser with a calcium chloride drying tube and a thermometer, and stir with a magnetic stirrer. Add 100mL xylene and 59.5g (0.2mol) bis(trichloromethyl)carbonate (BTC) into a three-necked flask, cool to below 0°C in an ice bath, stir, add 99.0g (0.5mol) 3,5-bis The mixture of chloro-2,4-difluoroaniline and 50 mL of xylene was slowly dropped, and the dropping temperature was controlled at 5-10°C. After the dropping, the temperature was raised to 90°C and reacted for 3 hours. Naturally cool, slowly add a mixture of 78.6g (0.5mol) 2,6-difluorobenzamide and 50mL xylene, add dropwise and raise the temperature to 100℃ to react for 7h, stop the reaction, cool naturally, filter, and dry in vacuo to obtain 181.2g of white needle-like solid, namely the product 1-(3,5-dichloro-2,4-difluorophenyl)-3-(2,6-difluorobenzoyl)urea, the yield is 93.5%, Analyzed by high performance liquid chromatography, the purity was 98.3%...

Embodiment 2

[0022] The amount ratio of the feed materials is 3,5-dichloro-2,4-difluoroaniline: bis(trichloromethyl) carbonate is 1:0.5, and the other operations are the same as in Example 1. The yield was 94.2%, and the purity was 98.6% by high performance liquid chromatography.

Embodiment 3

[0024] The quantity ratio of the feed materials is 3,5-dichloro-2,4-difluoroaniline: bis(trichloromethyl) carbonate is 1:0.6, and the other operations are the same as in Example 1. The yield was 94.7%, and the purity was 98.7% by high performance liquid chromatography.

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Abstract

The present invention relates to a preparation method of benzoyl urea derivative. In particular, it relates to a chemical synthesis method for preparing benzoyl urea derivative by using bis (trichloromethyl) carbonate instead of phosgene, diphosgene or oxalyl chloride to directly react with substituted aniline and substituted benzamide. Its reaction temperature is 20-200deg.C and reaction time is 1-20h.

Description

(1) Technical field [0001] The invention relates to a preparation method of benzoylurea derivatives, in particular to the use of bis(trichloromethyl) carbonate instead of phosgene, diphosgene or oxalyl chloride to directly react with substituted anilines and substituted benzamides to prepare benzene The chemical synthesis method of formyl urea derivatives. (2) Background technology [0002] Prior to the present invention, the existing process for chemically synthesizing benzoyl urea derivatives was to synthesize substituted benzoyl isocyanate from substituted benzamide and phosgene or oxalyl chloride, and then react with substituted aniline to generate benzoyl urea derivatives. For example: US4622340 (1986), US 6022882 (2000), Chemical Engineer, 2005, 115(4): 55 and so on. In current industrial production, substituted benzamide and excess oxalyl chloride are refluxed in 1,2-dichloroethane for several hours, and then the solvent and unreacted oxalyl chloride are removed by vacuum ...

Claims

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Application Information

Patent Timeline
31 Jan 2007
Publication
CN1903838A
IPC
C07C275/54
Inventors
贾建洪; 董华青