反应详情

温度

50 °C

To a solution of 302 mg crude 6-chloro-2-methoxy-4-methyl-pyridine-3-carboxylic acid in THF (12 ml) were added 568 mg (1.5 mmol) HATU and 934 μl (6.8 mmol) NEt3. The RM was stirred at 50° C. for 3 h followed by the addition of 268 mg (1.9 mmol) 3,5-difluorobenzylamine. Stirring was continued at 50° C. for 72 h. The RM was then diluted with EtOAc (50 ml) and subsequently washed with a 4M aq. NH4Cl sol., a 1M aq. NaHCO3 sol. and brine. The organic layer was dried over MgSO4 and concentrated in vacuo. Purification of the residue by CC (hexane/EtOAc 3:1) provided 237 mg (0.7 mmol, 54% over 2 steps) 2-methoxy-4-methyl-6-morpholin-4-yl-pyridine-3-carboxylic acid.

1. stirringStirring
2. waitwas continued at 50° C. for 72 h
3. washsubsequently washed with a 4M aq. NH4Cl sol.
4. dry with materialThe organic layer was dried over MgSO4
5. concentrationconcentrated in vacuo
6. customPurification of the residue by CC (hexane/EtOAc 3:1)