反应详情

Mixture of 2-bromo-7-acetoxy-3-(3,4,5-trimethoxybenzoyl)-6-methoxy-benzofuran (50 mg, 0.10 mmol) and methylacrylate (0.5 mL, excess) in a mixture of acetonitrile: TEA; 1 mL:0.5 mL was degassed with nitrogen and palladium acetate (10 mg) was added to it. Reaction mixture was stirred for one hour under nitrogen at reflux, more palladium acetate (15 mg) was added and the refluxing was continued for 7 hours (monitored by tlc). Methanol (1 mL) was added followed by the addition of potassium carbonate (70 mg, 0.51 mmol) and stirring was continued for 1 hour. Solvent was distilled and the crude material was purified over silica gel column (eluent Hexane:diethylether; 1:1) to afford the title compound as yellow crystalline solid (17 mg, 37%); 1H NMR (300 MHz, CDCl3) δ 7.61(d, 1H, J=15.76 Hz), 7.14(s, 2H, benzoyl Hs), 6.98(d, 1H, J=8.64 Hz), 6.89(d, 1H, J=8.69 Hz), 6.81(d, 1H, J=15.78 Hz), 3.96(s, 3H, OMe), 3.95(s, 3H, OMe), 3.81(s, 6H, 2×OMe), 3.77(bs, 3H, OMe).

1. custom1 mL:0.5 mL was degassed with nitrogen and palladium acetate (10 mg)
2. additionwas added to it
3. customReaction mixture
4. temperatureat reflux
5. waitthe refluxing was continued for 7 hours
6. stirringstirring
7. waitwas continued for 1 hour
8. distillationSolvent was distilled
9. customthe crude material was purified over silica gel column (eluent Hexane:diethylether; 1:1)