反应详情

A solution of 5-bromo-3-bromomethyl-pyridin-2-ylamine hydrobromide (11.0 g, 31.7 mmol) and 2-amino-2-methyl-propionic acid methyl ester (5.80 g, 49.5 mmol) in DMF (220 mL) was treated with triethylamine (9.0 mL, 18.5 mmol). After stirring at room temperature for 3 d, the mixture was diluted with H2O (400 mL) and then extracted with EtOAc (4×200 mL). The combined organic layers were washed with H2O (3×100 mL) and brine (100 mL), dried over Na2SO4, filtered and the solvent was removed in vacuo. Purification by flash column chromatography (silica gel, CH2Cl2/MeOH, 99:1) gave the title compound (3.87 g, 40%) as a light yellow solid: MS (ESI) m/e 302 (M+H)+.

1. extractionextracted with EtOAc (4×200 mL)
2. washThe combined organic layers were washed with H2O (3×100 mL) and brine (100 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, 99:1)