反应详情

温度

50 °C

3 g (0.0095 mol) of N-(5-amino-2-chloro-4-fluorophenyl)-N[(chloromethyl)sulfonyl]acetamide were dissolved in 30 mL of ethanol and 30 mL of 25% sodium hydroxide solution. The mixture was stirred for 3 hours at 50° C. and then cooled to room temperature. 6 N hydrochloric acid was added with stirring and cooling until the solution had a pH of 5-6. The suspension was further cooled to 0-5° C., filtered, washed with water and dried to yield 2.4 g (92%) of the title compound as a solid melting at 103.5-105.5° C. Recrystallization from toluene raised the melting point to 105-106° C.

1. temperaturecooled to room temperature
2. stirringwith stirring
3. temperaturecooling until the solution
4. temperatureThe suspension was further cooled to 0-5° C.
5. filtrationfiltered
6. washwashed with water
7. customdried