反应详情

13.5 g of 2-chloro-4-methyl-5-(2,2,2-trifluoroethylthio)aniline was added dropwise to 30 ml of concentrated hydrochloric acid at room temperature, and to this mixture, an aqueous solution containing 3.8 g of sodium nitrite was added dropwise at from 0 to 5° C., and the mixture was stirred as it was for 1 hour to prepare a diazonium salt. 36 g of tin chloride dihydrate was dissolved in 250 ml of 6N hydrochloric acid, and to this mixed solution, the above aqueous diazonium salt solution was added dropwise at from 0 to 5° C., and the solution was further stirred at room temperature for 2 hours. Toluene was added, the solution was neutralized with an aqueous sodium hydroxide solution, the insolubles were filtered off, and the organic layer was washed with water and dried over anhydrous magnesium sulfate. The solvent was distilled off under reduced pressure to obtain 12.1 g of 2-chloro-4-methyl-5-(2,2,2-trifluoroethylthio)phenylhydrazine.

1. additionwas added dropwise at from 0 to 5° C.
2. stirringthe solution was further stirred at room temperature for 2 hours
3. filtrationthe insolubles were filtered off
4. washthe organic layer was washed with water
5. dry with materialdried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off under reduced pressure