反应详情

Compound 67 (80 mg, 0.197 mmol) was dissolved in methanol 15 mL, Pd/C 50 mg added, and the reaction stirred under hydrogen balloon for 6 h. The reaction was filtered through celite bed and washed with excess methanol. The organic layer was concentrated to get the crude. The crude was purified by flash chromatography using 100-200 mesh silica gel. The compound was eluted at 26% ethyl acetate in hexane as half white coloured solid compound 68. 1HNMR (400 MHz, CDCl3) δ ppm 8.64 (d, 1H), 7.91 (d, 1H), 7.22 (d, 2H), 6.83 (s, 1H), 3.89 (m, 7H), 3.65 (dd, 1H), 3.44 (m, 1H), 3.16 (m, 6H), 2.72 (dd, 1H); MS (ESI) m/z 407.0 (M+H).

1. filtrationThe reaction was filtered through celite bed
2. washwashed with excess methanol
3. concentrationThe organic layer was concentrated
4. customto get the crude
5. customThe crude was purified by flash chromatography
6. washThe compound was eluted at 26% ethyl acetate in hexane as half white coloured solid compound 68