反应详情

温度

90 °C

To a solution of 7-(3-trifluoromethyl-pyridin-2-yl)-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepin-4-ol (185 mg, 0.60 mmol) in CH3CN (2 mL) was added POCl3 (0.11 mL, 1.19 mmol). The reaction mixture was heated at 90° C. for 2 h. The mixture was cooled to rt, diluted with EtOAc, and quenched slowly with saturated (satd.) aq. NaHCO3. The combined organic layers were dried (Na2SO4) and concentrated. The crude residue was purified (FCC) to give the title compound (65 mg, 33%).

1. temperatureThe mixture was cooled to rt
2. customquenched slowly with saturated (satd.) aq. NaHCO3
3. dry with materialThe combined organic layers were dried (Na2SO4)
4. concentrationconcentrated
5. customThe crude residue was purified (FCC)