反应详情

To a solution of Intermediate A (83 g, 0.26 mol) in DMF (600 mL) were K2CO3 (58 g, 0.417 mol) and 1,1-difluoro-2-iodo-ethane (60 g, 0.313 mol). Then the mixture was stirred at room temperature overnight. TLC (CH2Cl2: MeOH=20:1) showed the reaction was complete. The mixture was concentrated and the solid was diluted with CH2Cl2 (500 mL). The slurry was filtered and the filtrate was concentrated to give crude product, which was purified via prep. SFC to give compound B-33-1 (41.1 g, 41.3%) as a white solid.

1. concentrationThe mixture was concentrated
2. additionthe solid was diluted with CH2Cl2 (500 mL)
3. filtrationThe slurry was filtered
4. concentrationthe filtrate was concentrated
5. customto give crude product, which
6. customwas purified via prep
7. customSFC to give compound B-33-1 (41.1 g, 41.3%) as a white solid