反应详情

To a solution of 3.7 g (purity: 83.4%, 11.7 mmol) of 4-chloromethyl-5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole in 20 ml of ethanol was added 0.8 g (11.1 mmol) of thiourea, followed by stirring at room temperature overnight and further heating and stirring at 50° C. for 1 hour. The solvent was removed by evaporation under reduced pressure and the residue was washed with n-hexane to obtain 3.8 g (yield: 96.4%) of 2-(5-difluoromethoxy-1-methyl-3-trifluoromethyl-1H-pyrazole-4-ylmethyl)-isothiourea hydrochloride as white crystals (melting point: 117 to 119° C.)

1. temperaturefurther heating
2. stirringstirring at 50° C. for 1 hour
3. customThe solvent was removed by evaporation under reduced pressure
4. washthe residue was washed with n-hexane