HRID66034

反应详情

EQUATION

反应方程式

HRID 66034 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 20.0 g of 8-amino-1,3,6-naphthalenetrisulfonic acid trisodium salt and 8.75 g of sodium acetate trihydrate in 180 ml of water at room temperature is added 12.0 g of 3-nitrosulfobenzoic anhydride with stirring. A 400 ml portion of water is added. The mixture is stirred at room temperature for 21/2 hours and then filtered. The filtrate is cooled, acidified with 2-3 ml of concentrated hydrochloric acid an diluted with ethanol. The pink solid is collected by filtration, washed with 85% ethanol, ether and dried. The filtrate is concentrated to a low volume and diluted with ethanol giving a second crop which is collected and combined with the first crop giving a total of 27.6 g of 8-(3-nitro-2-sulfobenzamido)-1,3,6-naphthalene trisulfonic acid tetrasodium salt.

WORKUP

后处理

  1. stirringThe mixture is stirred at room temperature for 21/2 hours
  2. filtrationfiltered
  3. temperatureThe filtrate is cooled
  4. additionan diluted with ethanol
  5. filtrationThe pink solid is collected by filtration
  6. washwashed with 85% ethanol, ether
  7. customdried
  8. concentrationThe filtrate is concentrated to a low volume
  9. additiondiluted with ethanol giving a second crop which
  10. customis collected