反应详情

A mixture of intermediate (3) (0.041 mol), benzylamine (0.041 mol) and NaHCO3 (0.11 mol) in dioxane (100 ml) was stirred and refluxed for 48 hours. The solvent was evaporated. The residue was taken up in water and DCM. The separated organic layer was dried, filtered and the solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5). The desired fractions were collected, the solvent was evaporated, yielding (S)-2,3-dihydro-N-(phenylmethyl)-[1,4]dioxino[2,3-b]pyridine-3-methanamine (intermediate 55).

1. temperaturerefluxed for 48 hours
2. customThe solvent was evaporated
3. customThe separated organic layer was dried
4. filtrationfiltered
5. customthe solvent was evaporated
6. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 95/5)
7. customThe desired fractions were collected
8. customthe solvent was evaporated