HRID432048

反应详情

EQUATION

反应方程式

HRID 432048 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

Zink (38 g, 0.58 mol) was suspended in acetic acid (400 mL). The mixture was heated to 60° C. 2,4-dicarboxy-4′-fluoro-benzophenone (21 g, 0.075 mol) was added in portions of 5 grams. After addition, the reaction mixture was heated at reflux temperature for two hours. The suspension was filtered while it was still hot. The filtrate was added to ice-water (1 kg) and the title compound was isolated by filtration. Yield 17.8 g (90%). 1H NMR (d6-DMSO): δ 6.84 (s, 1H), 7.17 (t, 2H), 7.43 (dd, 2H), 7.59 (d, 1H), 8.31 (d, 1H), 8.35 (s, 1H).

WORKUP

后处理

  1. additionAfter addition
  2. temperaturethe reaction mixture was heated
  3. temperatureat reflux temperature for two hours
  4. filtrationThe suspension was filtered while it
  5. additionThe filtrate was added to ice-water (1 kg)