反应详情

A suspension of 2-(5-chloro-2-fluorophenyl)-5,7-dihydrofuro[3,4-d]pyrimidin-4-ol (100 mg, 0.36 mmol, 1 eq) in POCl3 (5 ml) was stirred under reflux for 1 h. The solution was then cooled to room temperature and concentrated under reduced pressure to give a white solid which was dissolved in dry methylene chloride. The solution was cooled to 0° C. and ice was added followed by sat. NaHCO3. The organic layer was separated, washed with brine, dried (MgSO4), filtered and evaporated in vacuo to provide a crude white solid which was purified by flash column chromatography (1:9 EtOAc:Hexane) to give 4-Chloro-2-(5-chloro-2-fluorophenyl)-5,7-dihydrofuro[3,4-d]-pyrimidine (78 mg, 73%) as a white solid.

1. temperatureunder reflux for 1 h
2. concentrationconcentrated under reduced pressure
3. customto give a white solid which
4. temperatureThe solution was cooled to 0° C.
5. additionice was added
6. customThe organic layer was separated
7. washwashed with brine
8. dry with materialdried (MgSO4)
9. filtrationfiltered
10. customevaporated in vacuo
11. customto provide a crude white solid which
12. customwas purified by flash column chromatography (1:9 EtOAc:Hexane)