反应详情

A mixture of crude 5-(3,5-Bis-trifluoromethyl-benzylamino)-7-bromo-8-chloro-2,3,4,5-tetrahydro-benzo[b]azepine-1-carboxylic acid isopropyl ester (1.40 g, 2.38 mmol) and pyridine (5.00 ml) was treated with acetic anhydride (5.00 ml) via dropwise addition. The mixture was stirred at room temperature overnight and then diluted with ethyl acetate (50.0 ml), washed with 1.00N HCl (2×50.0 ml) and brine (3×150 ml). Dried over Na2SO4, filtered and concentrated. Purification by silica gel chromatography (gradient eluent, 0-40% ethyl acetate in hexane) provided the titled compound (1.28 g, 85%) as white foamy solid. MS (ES+): 629, 631 (M+H).

1. washwashed with 1.00N HCl (2×50.0 ml) and brine (3×150 ml)
2. dry with materialDried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customPurification by silica gel chromatography (gradient eluent, 0-40% ethyl acetate in hexane)