HRID1654249

反应详情

EQUATION

反应方程式

HRID 1654249 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4,4'-Dimethoxybenzil (10 g), 90 ml glacial acetic acid and 160 ml 48% HBr were heated at reflux for 4 hours. The reaction mixture was poured into ice and the product collected by filtration. Dissolution of the solid into 10% aqueous sodium hydroxide, extraction with diethyl ether and acidification of the aqueous layer gave 4,4'-dihydroxybenzil which was recrystallized from 75% ethanol. Yield 7.5 g (84%). 1H NMR (acetone-d6) δ9.53 (s,2H, OH), 7.81, 6.98 (m, 8H, aromatic).

WORKUP

后处理

  1. temperatureat reflux for 4 hours
  2. additionThe reaction mixture was poured into ice
  3. filtrationthe product collected by filtration
  4. dissolutionDissolution of the solid
  5. extractioninto 10% aqueous sodium hydroxide, extraction with diethyl ether and acidification of the aqueous layer