反应详情

温度

0 °C

NaH, 60% (2.2 g; 0.0550 mol) was stirred in THF (170 ml) on an ice bath under N2. Intermediate D1 (19.3 g; 0.500 mol) was then added and stirred for 1 hour at 0° C. CH3I (7.8 g; 0.0550 mol) was then added and the reaction mixture was allowed to warm to room temperature overnight. Water was added and the THF was evaporated in vacuo. The precipitate was filtered off, washed with water and dried. Yield: 22.86 g of intermediate D2.

1. temperatureto warm to room temperature overnight
2. customthe THF was evaporated in vacuo
3. filtrationThe precipitate was filtered off
4. washwashed with water
5. customdried