反应详情

温度

20 °C

53 g of sodium nitrite was added to 300 ml of concentrated sulfuric acid at 50° C. or lower, and 300 ml of acetic acid was added dropwise at 50° C. or lower. To this mixed solution, 100 ml of an acetic acid solution of 182 g of 2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)aniline was added dropwise over a period of 2 hours at 20° C. or lower, followed by stirring at 20° C. for 3 hours. The reaction mixture was added dropwise at 5° C. or lower to a mixed solution of 390 g of tin(II)chloride dihydrate and 1,000 ml of 6N hydrochloric acid, followed by stirring for 30 minutes. Toluene was added to this reaction mixture, and the reaction mixture was neutralized with a 10% aqueous sodium hydroxide solution. The insolubles were filtered off, and the organic layer was dried over anhydrous magnesium sulfate and concentrated under reduced pressure to obtain 177 g of 2-fluoro-4-methyl-5-(2,2,2-trifluoroethylthio)phenylhydrazine.

1. stirringby stirring for 30 minutes
2. filtrationThe insolubles were filtered off
3. dry with materialthe organic layer was dried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure