HRID19970

反应详情

EQUATION

反应方程式

HRID 19970 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To dry methanol (20 ml) was carefully added thionyl chloride (1 ml) dropwise with stirring. The 3,4-diaminobenzoic acid (1 g) was added in portions at R.T. with stirring then the mixture heated at reflux for 3 h. Saturated sodium bicarbonate was added until the mixture was basic, then the mixture extracted into chloroform containing 25% methanol. The extract was dried and evaporated in vacuo to give the product (0.88 g, 81%) as a brown crystalline solid.

WORKUP

后处理

  1. stirringwith stirring
  2. temperaturethe mixture heated
  3. temperatureat reflux for 3 h
  4. extractionthe mixture extracted into chloroform containing 25% methanol
  5. customThe extract was dried
  6. customevaporated in vacuo