反应详情

A solution of 2-[(2-amino-5-bromo-pyridin-3-ylmethyl)amino]-2-methylpropionic acid methyl ester (2.63 g, 8.71 mmol) in DMSO (100 mL) was treated with NaH (60% dispersion in mineral oil, 0.35 g, 8.7 mmol). After stirring at room temperature overnight, the mixture was diluted with H2O (200 mL) and then extracted with EtOAc (5×150 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 to 98:2) gave (0.79 g, 33%) as an off-white solid: MS (ESI) m/e 270 (M+H)+.

1. extractionextracted with EtOAc (5×150 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 to 98:2)
7. customgave (0.79 g, 33%) as an off-white solid