反应详情

A suspension of compound 33.3 (0.136 mmol) in toluene was refluxed for 16 h. After removing the solvent, the residue was purified using silica gel column chromatography (TFA/Dichloromethane/ethyl acetate=1/5/40) to give compound 33 as a white solid (0.088 mmol). MS ESI m/e: 339 (M−H) 1H NMR (500 MHz) (DMSO-d6) δ 11.97 (1H, s); 7.31 (1H, t, J=10 Hz); 7.14 (2H, d, J=11 Hz); 6.99 (2H, m); 6.87 (3H, m); 5.22 (1H, s). 5.03 (2H, s); 3.75 (1H, m); 3.75 (3H, s); 2.44-2.53 (2H, m); 1.63 (3H, s); 1.62 (3H, s).

1. temperaturewas refluxed for 16 h
2. customAfter removing the solvent
3. customthe residue was purified