反应详情

温度

20 °C

0.95 g of N-(3-dimethylaminopropyl)-N′-ethylcarbodiimide in solution in 20 cm3 of dichloromethane is added, at 20° C., to 1.0 g of 4-morpholinobutyric acid, 0.78 g of ethyl isonipecotate, 2.1 cm3 of triethylamine and 20 mg of hydroxybenzotriazole hydrate, in solution in 80 cm3 of dichloromethane. After stirring for 20 hours at 20° C., the reaction mixture is washed with 20 cm3 of water. The organic phase is dried over magnesium sulfate, filtered and concentrated to dryness under reduced pressure (2.7 kPa) to give a pale yellow oil which is purified by chromatography on a CBT1 alumina column [eluent: dichloromethane/methanol (97/3 by volume)]. 1.30 g of ethyl 1-(4-morpholin-4-ylbutyryl)-4-piperidinecarboxylate are thus obtained in the form of a pale yellow oil.

1. washthe reaction mixture is washed with 20 cm3 of water
2. dry with materialThe organic phase is dried over magnesium sulfate
3. filtrationfiltered
4. concentrationconcentrated to dryness under reduced pressure (2.7 kPa)
5. customto give a pale yellow oil which
6. customis purified by chromatography on a CBT1 alumina column [eluent: dichloromethane/methanol (97/3 by volume)]