反应详情

In methanol (15 ml) were dissolved 2-amino-5-chloro-α-(3-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol produced in Example 1-(2) (0.6 g) and 3-benzyloxybenzaldehyde (0.38 g). To the solution was added acetic acid (0.12 g). To the mixture was added dropwise, while stirring at room temperature, cyano sodium borohydride (0.13 g). The reaction mixture was stirred for one hour at 60° C., to which was then added water (50 ml), followed by extraction with ethyl acetate (80 ml). The organic layer was 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-(3-benzyloxybenzyl)-5-chloro-α-(3-tert-butoxycarbonylaminomethylphenyl)benzyl alcohol (0.9 g) as a colorless oily product.

1. additionTo the mixture was added dropwise
2. stirringThe reaction mixture was stirred for one hour at 60° C., to which
3. extractionadded water (50 ml), followed by extraction with ethyl acetate (80 ml)
4. washThe organic layer was washed with water
5. dry with materialdried over anhydrous sodium sulfate
6. distillationThe solvent was distilled off
7. customthe residue was purified by means of a silica gel column chromatography