反应详情

温度

-10 °C

A solution of 554 g of the compound of Example 4 in 5 L of dichloromethane was cooled to -40° C. and 79 g of anhydrous ammonia was added at this temperature. The reaction mixture was allowed to warm to -10° C., stirred 1 hour, then poured into 6 L of water. The organic phase was separated and filtered. The filter cake was washed with dichloromethane and dried giving 356 g of crude product. A 180 g portion was recrystallized from methanol to give 130 g of the title compound, m.p. 139°-142° C.

1. customThe organic phase was separated
2. filtrationfiltered
3. washThe filter cake was washed with dichloromethane
4. customdried
5. customgiving 356 g of crude product
6. customA 180 g portion was recrystallized from methanol