反应详情

温度

0 °C

1907 g (11.48 mol) of 5-trifluoromethyl-3-hydroxy-1-methylpyrazole was stirred with 8 kg of ether and cooled to 0° C. 1222 g (6.2 mol) of 1,3-dichloro-5,5-dimethylhydantoin was added in three equal portions and the mixture was allowed to cool to 0° C. after each addition. The mixture was stirred for 4 hours, washed with water, brine and water. All washes were extracted with ether and the combined ether solutions were dried with MgSO4 filtered, evaporated on a rotary evaporator and recrystallized from methylcyclohexane to give 2131 g of a tan solid, m.p. 136°-140° C.

1. temperatureto cool to 0° C.
2. additionafter each addition
3. washwashed with water, brine and water
4. extractionAll washes were extracted with ether
5. dry with materialthe combined ether solutions were dried with MgSO4
6. filtrationfiltered
7. customevaporated on a rotary evaporator
8. customrecrystallized from methylcyclohexane