反应详情

A solution of 2-amino-2-fluoromethyl-3-(3-benzyloxy-4-methoxyphenyl)propionitrile (0.7 g) in absolute methanol saturated with dry hydrogen chloride (50 ml) is heated at reflux for 12 hours. The methanol is evaporated and the residue dissolved in trifluoroacetic acid (10 ml). The mixture is heated at reflux temperature for 2 hours. Water (4 ml) is then added, and reflux continues overnight. The residue obtained upon evaporation under reduced pressure is passed through Amberlite 120 H+ ion exchange resin column. The ninhydrin positive fractions are pooled and concentrated. The residue is crystallized from water-methanol-ether to afford the desired product.

1. temperatureat reflux for 12 hours
2. customThe methanol is evaporated
3. dissolutionthe residue dissolved in trifluoroacetic acid (10 ml)
4. temperatureThe mixture is heated
5. temperatureat reflux temperature for 2 hours
6. additionWater (4 ml) is then added
7. temperaturereflux
8. customThe residue obtained upon evaporation under reduced pressure
9. concentrationconcentrated
10. customThe residue is crystallized from water-methanol-ether