反应详情

温度

115 °C

7-Trifluoromethyl-pyrido[3,2-d]pyrimidin-4-ol (300 mg, 1.39 mmol) was dissolved in toluene (5 ml). DIPEA (541 mg, 4.18 mmol) and POCl3 (641 mg, 4.18 mmol) were added and the reaction mixture was heated to 115° C. (external temperature). The reaction was cooled to rt and partioned between water (50 ml) and EtOAc (50 ml). The phases were separated and the aq phase was extracted twice with EtOAc (25 ml). The combined organic layer was washed with NaHCO3 solution and brine, treated with MgSO4 and filtered. The filtrate was concentrated, redissolved in DCM and filtered over silica and again concentrated to give the desired product as a colorless solid.

1. temperatureThe reaction was cooled to rt
2. customThe phases were separated
3. extractionthe aq phase was extracted twice with EtOAc (25 ml)
4. washThe combined organic layer was washed with NaHCO3 solution and brine
5. additiontreated with MgSO4
6. filtrationfiltered
7. concentrationThe filtrate was concentrated
8. dissolutionredissolved in DCM
9. filtrationfiltered over silica
10. concentrationagain concentrated