反应详情

LiOH.H2O (25 mg, 0.6 mmole) was added to a solution of methyl (R)-8-[3-(2-pyridylamino)-1-propyloxy]-3-oxo-2-(2,2,2-trifluoroethyl)-2,3,4,5-tetrahydro-1H-2-benzazepine-4-acetate (0.25 g, 0.54 mmole) in THF (5 mL) and H2O (2 mL) at RT. After 18 hr, the reaction was concentrated to dryness and the residue was dissolved in H2O (4 mL). The solution was carefully brought to pH≈4 with 3.0 N HCl. The precipitate was collected and dried in high vacuum at 40-45° C. to afford the title compound (0.15 g, 62%) as an off-white solid: MS (ES) m/e 452.1 (M+H)+. Anal. Calcd for C22H24F3N3O4. 0.5 H2O: C, 57.38; H, 5.47; N, 9.12. Found: C, 57.72; H, 5.24; N, 8.92.

1. concentrationthe reaction was concentrated to dryness
2. dissolutionthe residue was dissolved in H2O (4 mL)
3. customThe precipitate was collected
4. customdried in high vacuum at 40-45° C.