反应详情

To a mixture of 5-chloro-1,3-dimethoxybenzene (25 g, 0.14 mol) in DMF (175 mL, 2.27 mol) at 0° C. was added POCl3 (42.5 mL, 0.46 mol) dropwise. The mixture was stirred at room temperature for 30 min and heated to reflux at 100° C. for an additional 2 h. The reaction mixture was poured onto ice and the yellow precipitate was collected by filtration, rinsed with cold water and dried under high vacuum to give a light yellow solid (22.7 g. Yield 78.3%). 1H NMR (400 MHz, CDCl3) δ0.43 (s, 1H), 6.59 (s, 1H), 6.42 (s, 1H), 3.92 (s, 3H), 3.89 (s, 3H); MS (ESI) m/z=201 [M+H]+.

1. temperatureheated
2. temperatureto reflux at 100° C. for an additional 2 h
3. additionThe reaction mixture was poured onto ice
4. filtrationthe yellow precipitate was collected by filtration
5. washrinsed with cold water
6. customdried under high vacuum
7. customto give a light yellow solid (22.7 g. Yield 78.3%)