HRID1393831

反应详情

EQUATION

反应方程式

HRID 1393831 反应方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

A mixture of sodium 2-[(4-nitrophenyl)amino]ethanesulfonate (8) (5.36 g, 0.02 mol), phosphorus pentachloride (4.58 g, 0.022 mol) and 50 mL of anhydrous xylene was heated at about 40-50° C. for 4 hours. After remaining at room temperature overnight, the mixture was heated for 3 hours in a boiling water bath. The resulting mixture was filtered while hot and the insoluble matter was washed three times with hot xylene. The filtrate was left to cool. A yellow solid formed, and was filtered off and reslurried in water. 2.4 g of expected product were isolated.

WORKUP

后处理

  1. temperaturethe mixture was heated for 3 hours in a boiling water bath
  2. filtrationThe resulting mixture was filtered while hot and the insoluble matter
  3. washwas washed three times with hot xylene
  4. waitThe filtrate was left
  5. temperatureto cool
  6. customA yellow solid formed
  7. filtrationwas filtered off