反应详情

To a solution of benzyl 4-(benzyloxy)-2-(1H-pyrazol-1-yl)pyrimidine-5-carboxylate, 2-d, (2 g crude) in EtOH(20 ml)/THF (20 ml)/water (20 ml) was added KOH (0.87 g, 15.5 mmol). The mixture was stirred at room temperature for 12 hours. The mixture was then concentrated under vacuum and the residue was diluted with water and basified to pH=2 with HCl followed by extraction with ethyl acetate. The organic layer was brine washed, dried over sodium sulfate and concentrated under vacuum. The residue was purified on a silica gel column with the eluent of petroleum ether/ethyl acetate=7/1 to afford the compound 2-e (200 mg, 13%).

1. concentrationThe mixture was then concentrated under vacuum
2. additionthe residue was diluted with water and basified to pH=2 with HCl
3. extractionfollowed by extraction with ethyl acetate
4. washwashed
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under vacuum
7. customThe residue was purified on a silica gel column with the eluent of petroleum ether/ethyl acetate=7/1