反应详情

Borane-tetrahydofuran complex (1.0 M in THF, 970 mL, 970 mmol) was added dropwise to a stirred solution of methyl (±)-(cis)-(7-bromo-8-fluoro-1,3,4,14b-tetrahydro-4-oxo-2H-dibenzo[b,f]pyrido[1,2-d][1,4]oxazepin-1-yl)carbamate (105.2 g, 242 mmol) in THF (1 L). The resulting mixture was stirred at ambient temperature for 3 h. Subsequently, hydrochloric acid (1M) was added dropwise until evolution of gas ceased (±550 mL). The resulting mixture was stirred for 1 h and then diluted with ethyl acetate; the organic layer was washed with water and brine. After drying (MgSO4) the solvent was evaporated under reduced pressure to yield the crude title compound (98.5 g, 97%). (m/z)=421+423 (M+H)+.

1. stirringThe resulting mixture was stirred for 1 h
2. washthe organic layer was washed with water and brine
3. dry with materialAfter drying (MgSO4) the solvent
4. customwas evaporated under reduced pressure