反应详情

Ethyl 4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylate, 11-b, (150 g, 0.46 mol) in THF (1.5 L) was treated with LiOH monohydrate (58 g, 1.39 mol) in water (60 ml) at room temperature for 3 hours. The mixture was concentrated under vacuum and diluted with water (200 ml) followed by extraction with ethyl acetate. The aqueous layer was acidified to pH=2 with 10% HCl and solid crashed out from the solution which was then filtered and washed with water to afford the product, 11-c, (40 g, 29%).

1. concentrationThe mixture was concentrated under vacuum
2. additiondiluted with water (200 ml)
3. extractionfollowed by extraction with ethyl acetate
4. filtrationwas then filtered
5. washwashed with water