反应详情

Reflux a mixture of 2-methoxymethyl-7-(3-trifluoromethyl-pyridin-2-yl)-3H-pyrido[2,3-d]pyrimidin-4-one (0.500 g, 1.49 mmol), 2,6-lutidine (0.69 mL), and POCl3 (0.555 mL) in CHCl3 (10 mL) for 5 hours. Cool the mixture and concentrate under reduced pressure. Partition the residue between EtOAc and saturated NaHCO3 solution. Wash the EtOAc portion with additional NaHCO3 and then dry (MgSO4) and concentrate under reduced pressure. Purified the crude by flash column chromatography on a silica gel (EtOAc eluent) and concentrate under reduced pressure to give 4-chloro-2-methoxymethyl-7-(3-trifluoromethyl-pyridin-2-yl)-pyrido[2,3-d]pyrimidine as a white solid.

1. temperatureReflux
2. temperatureCool the mixture
3. concentrationconcentrate under reduced pressure
4. customPartition the residue between EtOAc and saturated NaHCO3 solution
5. washWash the EtOAc portion with additional NaHCO3
6. dry with materialdry (MgSO4)
7. concentrationconcentrate under reduced pressure
8. customPurified the crude by flash column chromatography on a silica gel (EtOAc eluent)
9. concentrationconcentrate under reduced pressure