HRID485216

反应详情

EQUATION

反应方程式

HRID 485216 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
42 °C

PROCEDURE

实验过程

To a suspension of 3-sulphobenzoic acid (5 g, 2.5×10-2 moles) in dichloromethane (60 ml) containing a trace of sulphuric acid (5×10-5 moles) was slowly added hydrogen peroxide (3 g; 85%). The suspension was boiled under reflux (42° C.) for 1 hour after which it was cooled to room temperature, the dichloromethane was decanted off and the residue treated with saturated aqueous magnesium nitrate (25 ml). The resultant precipitate was filtered off, dried over phosphorous pentoxide under vacuum to yield the magnesium salt of 3-sulphoperoxybenzoic acid (3.5 g; 5.31% Avox as O; Magnesium content of 4.7%) compared with a theoretical yield of 5.67 g. The IR spectrum was again substantially the same as for the other preparations.

WORKUP

后处理

  1. temperaturewas cooled to room temperature
  2. customthe dichloromethane was decanted off
  3. additionthe residue treated with saturated aqueous magnesium nitrate (25 ml)
  4. filtrationThe resultant precipitate was filtered off
  5. dry with materialdried over phosphorous pentoxide under vacuum