HRID918605

反应详情

EQUATION

反应方程式

HRID 918605 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
90 °C

PROCEDURE

实验过程

A mixture of 4-chloro-3-nitro-5-sulphamyl-benzoic acid (14 g), p-methoxyphenol (9.3 g), and 1N sodium bicarbonate (200 ml) was stirred at 90°C for 5 hours. After cooling, the resulting 4-(p-methoxyphenoxy)-3-nitro-5-sulphamyl-benzoic acid was precipitated by the addition of 4N hydrochloric acid until the pH was 1, and collected by suction. The crude acid was dissolved in hot methanol (100 ml) and precipitated by the addition of water (100 ml) and cooling. After collection and drying in vacuo, the melting point was 229°-230°C.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe resulting 4-(p-methoxyphenoxy)-3-nitro-5-sulphamyl-benzoic acid was precipitated by the addition of 4N hydrochloric acid until the pH was 1
  3. customcollected by suction
  4. dissolutionThe crude acid was dissolved in hot methanol (100 ml)
  5. customprecipitated by the addition of water (100 ml)
  6. temperaturecooling
  7. customAfter collection
  8. customdrying in vacuo