反应详情

温度

60 °C

To a solution of phosphorous oxychloride (3.00 mL, 0.033 mol) in DMF (10 mL) was added a solution of 1-methoxy-3,4-methylenedioxybenzene (2.00 g, 0.013 mol) in DMF (2 mL) at 0° C. After stirring at 60° C. for 18 h the mixture was cooled to 0° C. and then poured into water (500 mL). The precipitate was filtered and dried. The title compound was collected as a yellow solid (2.20 g, 92%): 1H NMR (250 MHz, CDCl3) δ 10.22 (s, 1H), 7.20 (s, 1H), 6.52 (s, 1H), 5.98 (s, 2H), 3.85 (s, 3H); mp: 110°l C.

1. temperaturewas cooled to 0° C.
2. filtrationThe precipitate was filtered
3. customdried
4. customThe title compound was collected as a yellow solid (2.20 g, 92%)