反应详情

Heat a mixture of (R)-methanesulfonic acid 2-tert-butoxycarbonylamino-propyl ester (0.083 mol, 20 g) and morpholine (0.83 mol, 72.2 g) in acetonitrile (210 mL) to 65° C. for 16 h. Concentrate the reaction mixture, dilute the residue with water, extract with dichloromethane, combine organic layer and wash with water. Dry the organic layer over anhydrous sodium sulfate, filter and concentrate under vacuum to obtain the title compound (12 g, 62%) as yellow thick oil. 1H NMR (400 MHz, CDCl3) δ 1.13 (d, 3H), 1.43 (s, 9H), 2.21 (dd, 1H), 2.26-2.32 (m, 1H), 2.35-2.39 (m, 2H), 2.48-2.55 (m, 2H), 3.63-3.70 (m, 5H), 4.68 (br s, 1H, —NH).

1. temperatureHeat
2. concentrationConcentrate the reaction mixture
3. additiondilute the residue with water
4. extractionextract with dichloromethane
5. washwash with water
6. dry with materialDry the organic layer over anhydrous sodium sulfate
7. filtrationfilter
8. concentrationconcentrate under vacuum