反应详情

Diethylamine (13.8 g) was added dropwise over a period of 30 min to a mixture of benzoin (10 g) and malononitrile (3.8 g) in DMF (30 ml) at 0° C. (the internal temperature should not exceed 40° C.). After the resulting mixture was stirred at room temperature for 16 h, water (100 mL) was added. The resulting precipitate was filtered, washed with sufficient amount of water, then with hexanes, and dried. The solid was recrystallized from ethanol to provide yellowish-brown solid product of the title compound (6 g, 49%). 1H NMR (300 MHz, CDCl3): δ 7.47-7.34 (m, 8H), 7.28-7.18 (m, 2H), 4.94 (br, 2H). LC-MS (ESI) m/z 261.1 (M+H).

1. customexceed 40° C.
2. filtrationThe resulting precipitate was filtered
3. washwashed with sufficient amount of water
4. dry with materialwith hexanes, and dried
5. customThe solid was recrystallized from ethanol