反应详情

Intermediate (55) (0.0195 mol) was dissolved in ethanol (50 ml). 2-Propenenitrile (0.02 mol) was added and the reaction mixture was stirred and refluxed overnight. Additional 2-propenenitrile (0.02 mol) was added and the reaction mixture was stirred and refluxed for 2 hours. Additional 2-propenenitrile (0.02 mol) was added and the reaction mixture was stirred and refluxed for 6 hours. Additional 2-propenenitrile (0.02 mol) was added and the reaction mixture was stirred and refluxed overnight. The solvent was evaporated. The residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 97/3). The product fractions were collected and the solvent was evaporated, yielding 6.0 g of (S)-3-[[(2,3-dihydro[1,4]dioxino[2,3-b]pyridin-3-yl)methyl](phenylmethyl)amino]-propanenitrile (intermediate 56).

1. temperaturerefluxed overnight
2. stirringthe reaction mixture was stirred
3. temperaturerefluxed for 2 hours
4. stirringthe reaction mixture was stirred
5. temperaturerefluxed for 6 hours
6. stirringthe reaction mixture was stirred
7. temperaturerefluxed overnight
8. customThe solvent was evaporated
9. customThe residue was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH 97/3)
10. customThe product fractions were collected
11. customthe solvent was evaporated