反应详情

A mixture of the product of example 35B (0.516 g, 1.85 mmol), PdCl2dppf.CHCl3 (75 mg, 0.091 mmol), and triethylamine (0.39 mL, 2.8 mmol) was stirred in 1:1 DMF:MeOH (6 mL, pre-saturated with CO) under CO (1 atm) at 80° C. for 4 hours, diluted with EtOAc, washed with water and brine, dried (Na2SO4), and filtered. The residue was chromatographed on SiO2 (3-12% Et2O/hexanes) to give 112.0 mg of the title compound as a clear gum. 1H NMR (300 MHz, DMSO) δ 8.09 (dd, 1H), 7.62-7.69 (m, 3H), 7.49-7.57 (m, 3H), 7.45 (dd, 1H), 3.57 (s, 3H).

1. washwashed with water and brine
2. dry with materialdried (Na2SO4)
3. filtrationfiltered
4. customThe residue was chromatographed on SiO2 (3-12% Et2O/hexanes)