反应详情

To a solution of methyl 4-morpholinepropionate (5.0 g, 28.9 mmol) in MeOH (25 mL) was added 2N NaOH (17.3 mL, 34.6 mmol). The mixture was stirred for 1 h then concentrated in vacuo. The residue was suspended in dichloromethane (125 mL) and DMF (30 μL) was added followed by oxalylchloride (10 mL, 115.6 mmol). The mixture was allowed to stir for 2 h. then concentrated in vacuo. The resulting solid was added portion-wise to a solution of 2-(aminomethyl)pyridine (2.88 mL, 28.2 mmol) and triethylamine (9.0 mL, 64.86 mmol) in dichloromethane (200 mL). The mixture was stirred at ambient temperature for 1 h. then washed with water (300 mL). The organic layer was dried over anhydrous sodium sulfate and concentrated to yield 3-morpholin-4-yl-N-pyridin-2-ylmethyl-propionamide (5.56 g, 77%).

1. concentrationthen concentrated in vacuo
2. additionDMF (30 μL) was added
3. stirringto stir for 2 h.
4. concentrationthen concentrated in vacuo
5. stirringThe mixture was stirred at ambient temperature for 1 h.
6. washthen washed with water (300 mL)
7. dry with materialThe organic layer was dried over anhydrous sodium sulfate
8. concentrationconcentrated