反应详情

6-Methoxymethyl-3-(3-trifluoromethyl-pyridin-2-yl)-pyrido-[2,3-b]pyrazin-8-ol (146 mg, 0.436 mmol) is dissolved in a solution of CHCl3 (20 mL), POCl3 (0.12 ml, 1.31 mmol) and 2,6-lutidine (0.2 mL, 1.31 mmol). The mixture is heated at reflux overnight. The reaction is concentrated under reduced pressure. EtOAc (30 mL) is added and the mixture is extracted with NaHCO3 (aq) (30 mL) and brine (30 mL). The organic extract is dried over Na2SO4 and the solvent removed under reduced pressure. The crude product is purified by silica gel preparatory TLC eluting with hexanes/EtOAc (1:1) to yield the title compound as a light yellow oil that solidifies upon standing.

1. temperatureThe mixture is heated
2. temperatureat reflux overnight
3. concentrationThe reaction is concentrated under reduced pressure
4. additionEtOAc (30 mL) is added
5. extractionthe mixture is extracted with NaHCO3 (aq) (30 mL) and brine (30 mL)
6. extractionThe organic extract
7. dry with materialis dried over Na2SO4
8. customthe solvent removed under reduced pressure
9. customThe crude product is purified by silica gel preparatory TLC
10. washeluting with hexanes/EtOAc (1:1)