反应详情

Reflux a mixture of 2-isobutoxymethyl-7-(3-trifluoromethyl-pyridin-2-yl)-3H-pyrido[2,3-d]pyrimidin-4-one (0.510 g, 1.35 mmol), 2,6-lutidine (0.62 mL), and POCl3 (0.50 mL) in CHCl3 (10 mL) for 16 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 (Na2SO4) and concentrate under reduced pressure. Filter the brown residue through 2 inches of silica gel (1:1 EtOAc/hexanes eluent) and concentrate under reduced pressure to give 4-chloro-2-isobutoxymethyl-7-(3-trifluoromethyl-pyridin-2-yl)-pyrido[2,3-d]pyrimidine as yellow viscous oil.

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 (Na2SO4)
7. concentrationconcentrate under reduced pressure
8. filtrationFilter the brown residue through 2 inches of silica gel (1:1 EtOAc/hexanes eluent)
9. concentrationconcentrate under reduced pressure