HRID1085643

反应详情

EQUATION

反应方程式

HRID 1085643 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Into a 250 ml round bottom flask equipped with a magnetic stirrer and reflux condenser was placed 1,2-diaminobenzene (2.3275 g, 0.0215 mol), 4,4'-dihydroxybenzil (5.2135 g, 0.0215 mol) and absolute ethanol (30 ml). The solution was stirred for one-half hour at room temperature, and a yellow precipitate formed. The mixture was heated to reflux overnight. The solvent was removed by vacuum distillation and the solid dried at 100° C. for two hours to give 6.6 g (97%) of yellow powder. The material was recrystallized from 1,4-dioxane/water mixture. Yield 6.0 g (89%) m.p. 336° C.-338° C. Anal. Calcd for C20H14N2O2 : C, 76.42%; H, 4.49%; N, 8.91%. Found: C, 76.54%; H, 4.44%; N,8.96%.

WORKUP

后处理

  1. customInto a 250 ml round bottom flask equipped with a magnetic stirrer
  2. temperaturereflux condenser
  3. customa yellow precipitate formed
  4. temperatureThe mixture was heated
  5. temperatureto reflux overnight
  6. customThe solvent was removed by vacuum distillation
  7. customthe solid dried at 100° C. for two hours