反应详情

Intermediate c (9 g, 0.042 mol) was added to DMF (100 mL). To the mixture was added NaH (1.3 g, 0.054 mol) in batch under an ice bath. After stirring for 30 min, n-butyl bromide (3.4 mL, 0.042 mol) was added dropwise. After the dropwise addition, the reaction was conducted at 70° C. for 6 h. After completion of the reaction, the reaction solution was poured into water (600 mL). A great deal of solid separated out and was filtered by suction. The filtered cake was washed with water and dried to produce Intermediate f (8.2 g) in a yield of 81.4%.

1. additionAfter the dropwise addition
2. waitthe reaction was conducted at 70° C. for 6 h
3. customAfter completion of the reaction
4. customA great deal of solid separated out
5. filtrationwas filtered by suction
6. washThe filtered cake was washed with water
7. customdried