HRID727479

反应详情

EQUATION

反应方程式

HRID 727479 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

34.6 g (100 mmol) of dipotassium 2,5-dihydroxybenzene-1,4-disulfonate were dissolved in 500 ml of water at 60° C. After addition of 0.68 g (2 mmol) of iron 5,14-dihydrodibenzo[b,i][5,9,14,18]-tetraaza[14]annulene, 0.8 g (2 mmol) of diethylenetriaminepentaacetic acid, 1 ml of concentrated sulfuric acid and 1 ml of a commercial antifoam agent, 28.4 g (250 mmol) of 30% by weight aqueous hydrogen peroxide were added dropwise. The mixture was stirred for 15 min at 60° C. The solution was cooled to 5°-10° C. and then the solid was filtered off with suction and recrystallized from water to yield 14.5 g (42%) of dipotassium 1,4-benzoquinone-2,5-disulfonate in the form of reddish brown needles. Melting point >360° C.

WORKUP

后处理

  1. additionwere added dropwise
  2. temperatureThe solution was cooled to 5°-10° C.
  3. filtrationthe solid was filtered off with suction
  4. customrecrystallized from water