反应详情

Compound 1b (1.36 g, 5.98 mmol) was stirred in DMF (10 mL) at 88° C. Selectfluor® (2.54 g, 7.17 mmol) in DMF (8 ml) was added dropwise, and the reaction stirred for 1 h. Additional Selectfluor® (1.2 g, 3.39 mmol) in DMF (5 mL) was added, and the reaction stirred 1 h longer. The solution was concentrated in vacuo and purified by silica gel chromatography (75% EtOAc/CH2Cl2) to give 460 mg (31%) of compound 1c as a white solid. 1H NMR (400 MHz, CDCl3): δ 4.18 (t, 2H, J=7.6 Hz), 3.86 (s, 3H), 3.37 (t, 2H, J=7.6 Hz), 2.20-2.28 (m, 2H). MS (ES) [m+H] calc'd for C10H9ClFNO3, 246, 248. found 246, 248.

1. stirringthe reaction stirred 1 h longer
2. concentrationThe solution was concentrated in vacuo
3. custompurified by silica gel chromatography (75% EtOAc/CH2Cl2)