反应详情

温度

0 °C

2.9 g (9.5 mmol) of 6-amino1-[3-(4-cyano-phenyl)propionyl]-1,2,3,4-tetrahydro-quinoline are dissolved in 80 ml of methanol and 0.6 ml of acetic acid, combined with 1.06 g (10 mmol) of benzaldehyde and stirred for 20 minutes at 0° C. Then 0.63 g sodium cyanoborohydride are added in small batches, stirring is continued for half an hour and the mixture is then allowed to warm up to ambient temperature. The solution is then concentrated by rotary evaporation and the residue is taken up in a little ice water. Then the solution is acidified and sodium hydroxide solution is added until an alkaline reaction is obtained and the mixture is then extracted with me-thylene chloride. The dried solution is concentrated by rotary evaporation and the residue is chromatographed over a silica gel column with toluene/ethyl acetate (1:1).

1. stirringstirring
2. waitis continued for half an hour
3. temperatureto warm up to ambient temperature
4. concentrationThe solution is then concentrated by rotary evaporation
5. additionsodium hydroxide solution is added until an alkaline reaction
6. customis obtained
7. extractionthe mixture is then extracted with me-thylene chloride
8. concentrationThe dried solution is concentrated by rotary evaporation
9. customthe residue is chromatographed over a silica gel column with toluene/ethyl acetate (1:1)