反应详情

A solution of (2-Morpholin-4-yl-ethylamino)acetic acid methyl ester (0.40 g, 2.0 mmol) and triethylamine (1.0 mL, 7.11 mmol) in DMF (20 mL) was treated with 5-bromo-3-bromomethyl-pyridin-2-ylamine hydrobromide (0.70 g, 2.0 mmol). After stirring at room temperature under for 7 h, the cloudy mixture was diluted with H2O (50 mL) and then extracted with EtOAc (4×50 mL). The combined organic layers were washed with H2O (3×50 mL) and brine (50 mL), dried over Na2SO4, filtered and the solvent was removed in vacuo. Purification by flash column chromatography (silica gel, CH2Cl2/MeOH, 98:2 to 96:4) gave the title compound (0.46 g, 60%) as a colorless oil: MS (ESI) m/e 387 (M+H)+.

1. extractionextracted with EtOAc (4×50 mL)
2. washThe combined organic layers were washed with H2O (3×50 mL) and brine (50 mL)
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. customthe solvent was removed in vacuo
6. customPurification by flash column chromatography (silica gel, CH2Cl2/MeOH, 98:2 to 96:4)