反应详情

To a solution of (4-amino-3,5-diethoxy-phenyl)-methanol (0.79 g, 3.74 mmol, 1.0 equiv) in DMF (20 mL) was added activated MnO2 (1.63 g, 18.70 mmol, 5.0 equiv). The reaction mixture was stirred for 24 h at rt, filtered through Hyflo Super Cel, the filtrate was extracted with ethyl acetate (3×50 mL), and the combined organic phase was washed with water, dried over MgSO4 and evaporated to dryness providing thereby 0.69 g (88%) of the title compound. 1H NMR (300 MHz, DMSO): δ 1.46 (t, J=7.0 Hz, 3H), 4.15 (q, J=7.0 Hz, 2H), 4.50 (br s, 2H), 7.04 (s, 2H), 9.70 (s, 1H). MS (ISP): 210.0 [M+H]+.

1. filtrationfiltered through Hyflo Super Cel
2. extractionthe filtrate was extracted with ethyl acetate (3×50 mL)
3. washthe combined organic phase was washed with water
4. dry with materialdried over MgSO4
5. customevaporated to dryness
6. customproviding