反应详情

温度

50 °C

To a solution of 101g (40 g, 168 mmol) in glacial acetic acid (360 mL) was added hydrazine monohydrate (240 mL) at 0-10° C. under N2 protection. The resulting slurry was stirred under nitrogen at 50° C. for 1.5 hours. The reaction mixture was poured into 300 mL of water with continuous stirring. The aqueous phase was extracted with DCM (2×500 mL), and the combined organic phase was dried over Na2SO4, filtered and concentrated to give a residue, which was purified by re-crystallization in DMC and Et2O to provide 101h (17 g, 37.6% over 2 steps) as an off-white solid. 1HNMR (300 MHz, CDCl3) δ 8.11 (d, J=2.7 Hz, 1H), 7.46 (m, 2H), 1.39 (s, 9H). LCMS (ESI) m/z 221 (M+H)+.

1. extractionThe aqueous phase was extracted with DCM (2×500 mL)
2. dry with materialthe combined organic phase was dried over Na2SO4
3. filtrationfiltered
4. concentrationconcentrated
5. customto give a residue, which
6. customwas purified by re-crystallization in DMC and Et2O