反应详情

To a stirring solution of [4-(6{-3-[(2-Chloro-3-trifluoromethyl-benzyl)-(2,2-diphenyl-ethyl)-amino]-propoxy}-pyridin-2-yl)-piperazin-1-yl]-acetic acid methyl ester (46 mg, 0.07 mmol) in THF (2 ml) and H2O (0.5 ml) was added LiOH (6 mg, 0.13 mmol). The reaction mixture was stirred for 24 h at RT and then concentrated. The aqueous mixture was acidified to pH=3 with 1 N HCl (aq) and extracted with EtOAc (three times). The organic extracts were dried over Na2SO4, filtered, and concentrated. The free base was dissolved in dichloromethane and 1 N HCl (Et2O) was added. The solution was concentrated under vacuum to provide the title compound as a white solid, 26 mg (45%). MS (ESI) 667.2 (M+).

1. concentrationconcentrated
2. extractionextracted with EtOAc (three times)
3. dry with materialThe organic extracts were dried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated
6. dissolutionThe free base was dissolved in dichloromethane
7. addition1 N HCl (Et2O) was added
8. concentrationThe solution was concentrated under vacuum