反应详情

4-Chloro-2-methylsulfanyl-7-(3-trifluoromethyl-pyridin-2-yl)-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepine. To a solution of 2-methylsulfanyl-7-(3-trifluoromethyl-pyridin-2-yl)-6,7,8,9-tetrahydro-5H-pyrimido[4,5-d]azepin-4-ol (1.8 g, 4.92 mmol) in CH3CN (40 mL) was added POCl3 (1.4 mL, 14.8 mmol). After 15 min at 80° C., the mixture was cooled to rt, diluted with EtOAc, and quenched slowly with satd. aq. NaHCO3. The organic layer was separated, dried (MgSO4), and concentrated. The crude residue was purified (FCC) to give the title compound (1.6 g, 89%).

1. customquenched slowly with satd
2. customThe organic layer was separated
3. dry with materialdried (MgSO4)
4. concentrationconcentrated
5. customThe crude residue was purified (FCC)