HRID36539

反应详情

EQUATION

反应方程式

HRID 36539 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
15 °C

PROCEDURE

实验过程

4.00 g (0. 0149 mol) 5-sulfo isophtalic acid was dissolved in 11.00 g 98% sulfuric acid at 35° C. during 1 hour and was then cooled to 15° C. 3.58 g (0.895 mol) 85% hydrogen peroxide was added by drops, the temperature not exceeding 25° C. After 2 hours reaction at 35° C., 200 ml saturated Na2SO4 solution and a few grams of solid Na2SO4 were added. The solution was poured into cold tert.butylmethyl ether and was allowed to stand for 2 hours under agitation. The tert.butyl-methyl ether phase was separated and dried over Na2SO4, whereupon the solvent was evaporated and 5-sulfo diperoxy isophtalic acid precipitated as crystals. The yield of active oxygen was 80.6%.

WORKUP

后处理

  1. customexceeding 25° C
  2. customAfter 2 hours reaction at 35° C.
  3. customThe tert.butyl-methyl ether phase was separated
  4. dry with materialdried over Na2SO4, whereupon the solvent
  5. customwas evaporated
  6. custom5-sulfo diperoxy isophtalic acid precipitated as crystals