反应详情

To a cold solution (ice bath) of N-Boc-2-morpholinecarboxylic acid (0.5 g, 2.16 mmol) in DMF (10 mL) was added HATU ((2-(7-Aza-1H-benzotriazole-1-yl)-1,1,3,3-tetramethyluronium hexafluorophosphate) (0.98 g, 2.58 mmol), N,N diisopropylethylamine (2.2 g, 17.3 mmol), and 1 mL of 8 N solution of methylamine in ethanol. After the addition was finished the ice bath was removed, and the heterogeneous solution was stirred overnight at room temperature. The solution was dissolved in ethyl acetate (50 mL) and washed with a saturated solution of NaHCO3. Ethyl acetate layer was separated, dried (MgSO4) and concentrated under reduced pressure to give tert-butyl 2-(methylcarbamoyl)morpholine-4-carboxylate as an oil. MS (APCI) 245 (M+)

1. additionAfter the addition
2. customwas removed
3. dissolutionThe solution was dissolved in ethyl acetate (50 mL)
4. washwashed with a saturated solution of NaHCO3
5. customEthyl acetate layer was separated
6. dry with materialdried (MgSO4)
7. concentrationconcentrated under reduced pressure