反应详情

4-Iodo-m-xylene (4.31 mmol), triethyl phosphite (6.03 mmol) and palladium acetate (0.43 mmol) were mixed together in acetonitrile (10 ml), in a microwave tube. The vessel was sealed and placed in a microwave to react at 160° C., for 45 minutes. After cooling to room temperature, acetonitrile was removed. The crude material was purified by silica gel chromatography (eluent: stepwise gradient of ethyl acetate (0-30%) in petroleum ether) to yield Intermediate I.1 as an oil (84%). Intermediate 1.1 was characterized by the following spectroscopic data: 1H NMR (CDCl3, 400 MHz) δ (ppm) 1.32 (t, J=8.0 Hz, 6H), 2.35 (s, 3H), 2.53 (s, 3H), 4.07-4.14 (m, 4H), 7.07-7.08 (m, 2H), 7.77-7.83 (m, 1H); 31P NMR (CDCl3, 162 MHz) δ (ppm) 20.15 (s, 1P); and MS (ESI, EI+) m/z=243 (MH+).

1. customThe vessel was sealed
2. customto react at 160° C., for 45 minutes
3. customacetonitrile was removed
4. customThe crude material was purified by silica gel chromatography (eluent