HRID2072330

反应详情

EQUATION

反应方程式

HRID 2072330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

Water (20 parts) is set stirring and 2-hydroxy-3-naphthoic acid (9.5 parts) charged. Sodium hydroxide liquor (70° Tw -- 6.8 parts) is then added until an alkaline reaction is obtained on Brilliant Yellow test paper. 3-aminophenylphosphonic acid (8.7 parts) and sodium bisulphite liquor (40% -- 100 parts) are charged and the mixture is stirred and boiled under reflux for 18 hours. Carbon dioxide is evolved during the early part of the boiling period. After cooling to 80° C the suspension is acidified with hydrochloric acid (36% -- 59 parts) until acid reaction is obtained on Congo Red paper. During acidification the temperature is raised steadily to the boiling point and the suspension is boiled under reflux for 1-2 hours until evolution of sulphur dioxide has essentially ceased. During this period samples are spotted on to Congo Red test paper to confirm a positive acid reaction. The suspension is then cooled to room temperature, filtered and the cake washed with water (10 parts). The paste (18.2 parts) is dried an air at 50° C to give 12.9 parts of 2-(3-phosphonophenylamino)-naphthalene.

WORKUP

后处理

  1. customis obtained on Brilliant Yellow test paper
  2. temperatureunder reflux for 18 hours
  3. customis obtained on Congo Red paper
  4. temperatureDuring acidification the temperature is raised steadily to the boiling point
  5. customa positive acid reaction
  6. temperatureThe suspension is then cooled to room temperature
  7. filtrationfiltered
  8. washthe cake washed with water (10 parts)
  9. customThe paste (18.2 parts) is dried an air at 50° C