反应详情

温度

60 °C

In methanol (20 ml) were dissolved 2-amino-5-chloro-α-(3-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol (0.5 g) obtained in Example 1 (2) and 2-benzyloxybenzaldehyde (0.7 g). To the solution were added acetic acid (0.15 g) and cyano sodium borohydride (0.16 g). The mixture was stirred for 40 minutes at 60° C. The reaction mixture was concentrated, to which were added water (50 ml) and ethyl acetate (60 ml), followed by subjecting the mixture to extraction. The organic layer was separated, washed with water and dried over anhydrous sodium sulfate. The solvent was distilled off, and the residue was purified by means of a silica gel column chromatography to give 2-(2-benzyloxybenzylamino)-5-chloro-α-(3-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol (1.05 g) as a colorless oily product.

1. concentrationThe reaction mixture was concentrated, to which
2. additionwere added water (50 ml) and ethyl acetate (60 ml)
3. extractionto extraction
4. customThe organic layer was separated
5. washwashed with water
6. dry with materialdried over anhydrous sodium sulfate
7. distillationThe solvent was distilled off
8. customthe residue was purified by means of a silica gel column chromatography