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ChemicalBook CAS DataBase List 5-CHLORO-3-METHYL-1-PHENYLPYRAZOLE
1131-17-5

5-CHLORO-3-METHYL-1-PHENYLPYRAZOLE synthesis

5synthesis methods
-

Yield: 90.5%

Reaction Conditions:

with trichlorophosphate at 60 - 110; for 3 h;

Steps:

1 Compound B preparation process
In a dry four-necked flask, 184 g of phosphorus oxychloride was added.Then 172 g of compound C (3-methyl-1-phenyl-5-pyrazolone) was added,After stirring and stirring for 30 minutes, the temperature is raised to 60°C.Then let it naturally warm up to 80°C,Stay for 30 minutes,No longer warming upReheat to 110°C for 2 hours,Pour the material into 1500 ml waterIn the separatory funnel, separate the lower oil,3X100ml washed three times, the oil was vacuum distilled 3mm mercury 100-110 ° C to give 3-methyl-1-phenyl-5-chloropyrazole dry product 174 g,Content 99.5% (yield 90.5%).

References:

Jiangxi Kaiyuan Bio-pharmaceutical Technology Co., Ltd.;Xiangtan Kaiyuan Chemical Co., Ltd.;Chen Luwu;Zhou Zhijun CN107935933, 2018, A Location in patent:Paragraph 0033; 0034; 0035; 0036