反应详情

A solution of [(2-amino-5-bromo-pyridin-3-ylmethyl)amino]acetic acid ethyl ester (1.79 g, 6.21 mmol) in DMSO (70 mL) was treated with NaH (60% dispersion in mineral oil, 0.25 g, 6.2 mmol). After stirring at room temperature for 27 h, the mixture was diluted with H2O (300 mL), and extracted then with EtOAc (4×150 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 to give the title compound (1.09 g, 72%) as an off-white solid: 1H NMR (300 MHz, CDCl3) δ 8.26 (d, J=2.1 Hz, 1H), 8.17 (s, 1H), 7.54 (d, J=1.9 Hz, 1H), 4.03 (s, 2H), 3.93 (s, 2H), 1.85 (br s, 1H); MS (ESI) m/e 242 (M+H)+.

1. extractionextracted
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