HRID484555

反应详情

EQUATION

反应方程式

HRID 484555 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

10.1 g of aniline-2-sulphonic acid (85%) were dissolved in 40 ml of sodium hydroxide solution (6%) and treated with 40 ml of conc. HCl. 12 ml of aqueous NaNO2 solution were added dropwise to the resulting suspension at a temperature of 0° to 5° C. and the mixture was stirred at this temperature for 30 minutes. 50 g of sodium acetate, 300 ml of methanol and 0.5 g of bis(dibenzylideneacetone-2,2'-disulphonic acid disodium salt)palladium(0) were added successively and the mixture was stirred for 3 hours at 20° C. under an ethylene pressure of 20 bar. It was then filtered and evaporated to dryness, and the residue was stirred with ethanol. The mixture was again filtered and evaporated. 7.4 g (72%) of styrene-2-sulphonic acid, Na salt, were obtained.

WORKUP

后处理

  1. stirringthe mixture was stirred for 3 hours at 20° C. under an ethylene pressure of 20 bar
  2. filtrationIt was then filtered
  3. customevaporated to dryness
  4. stirringthe residue was stirred with ethanol
  5. filtrationThe mixture was again filtered
  6. customevaporated