反应详情

温度

70 °C

To a solution of (7RS)-7-(3,4-dichlorophenyl)-7-(methoxymethyl)-1,4-oxazepan-3-one (535 mg) in THF (10 ml) was added 1 M borane-THF solution (5 ml), and the mixture was stirred at 70° C. for 30 min. The reaction mixture was quenched with water, 2N hydrochloric acid (5 mL) was added, and the mixture was stirred at 70° C. for 10 min. The solvent was evaporated under reduced pressure, the residue was alkalified with potassium hydroxide, and the mixture was extracted three times with ethyl acetate. The organic layer was washed with brine, and dried over anhydrous sodium sulfate, and the solvent was evaporated. The residue was purified by silica gel column chromatography (NH, eluent; hexane:ethyl acetate (1:1)-(0:10)) to give the title compound as a free amine form (397 mg).

1. customThe reaction mixture was quenched with water, 2N hydrochloric acid (5 mL)
2. additionwas added
3. stirringthe mixture was stirred at 70° C. for 10 min
4. customThe solvent was evaporated under reduced pressure
5. extractionthe mixture was extracted three times with ethyl acetate
6. washThe organic layer was washed with brine
7. dry with materialdried over anhydrous sodium sulfate
8. customthe solvent was evaporated
9. customThe residue was purified by silica gel column chromatography (NH, eluent; hexane:ethyl acetate (1:1)-(0:10))