反应详情

温度

15 °C

A mixture of [3-(3-formyl-4-nitro-phenoxy)-phenyl]-carbamic acid benzyl ester (0.038 mol) in DCE (300 mL) was cooled in an ice bath to 15° C., then propylamine (0.042 mol), followed by NaBH(OAc)3 (0.057 mol) which was added portionwise. The reaction mixture was stirred overnight at room temperature and the mixture was washed with a saturated NaHCO3 solution. The organic layer was separated, dried (MgSO4), filtered off and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: 90:10 CH2Cl2:CH3OH). The product fractions were collected and the solvent was evaporated, then co-evaporated with toluene to yield the title compound as a residue.

1. additionwas added portionwise
2. washthe mixture was washed with a saturated NaHCO3 solution
3. customThe organic layer was separated
4. dry with materialdried (MgSO4)
5. filtrationfiltered off
6. customthe solvent was evaporated
7. customThe residue was purified by column chromatography over silica gel (eluent: 90:10 CH2Cl2:CH3OH)
8. customThe product fractions were collected
9. customthe solvent was evaporated