反应详情

A mixture containing (5-(tert-butoxycarbonylamino)pyridin-2-yl)methyl methanesulfonate (114; 1.70 g), morpholine (48; 1.0 g, 11.3 mmol) and K2CO3 (2.30 g, 16.9 mmol) in acetonitrile (30 mL) was stirred at room temperature for 12 h. Water (30 mL) was added and the mixture was extracted with ethyl acetate (3×30 mL). The combined organic layers were dried (MgSO4) and concentrated under reduced pressure. The resulting residue was purified by chromatography (petroleum ether:ethyl acetate=1:1 to 1:3) to afford tert-butyl 6-(morpholinomethyl)pyridin-3-ylcarbamate 115 (1.20 g, 71% for two steps).

1. extractionthe mixture was extracted with ethyl acetate (3×30 mL)
2. dry with materialThe combined organic layers were dried (MgSO4)
3. concentrationconcentrated under reduced pressure
4. customThe resulting residue was purified by chromatography (petroleum ether:ethyl acetate=1:1 to 1:3)