HRID450073

反应详情

EQUATION

反应方程式

HRID 450073 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

2-Chloro-5-nitrobenzoic acid (2 g, 9.9 mmol) was dissolved in of 8% sodium hydroxide solution (10 ml) at room temperature. 40% dimethyl amine aqueous solution (1.5 eq) was added and the reaction mixture was heated to reflux for 3 days. The reaction mixture was neutralized with dilute hydrochloric acid and extracted with ethyl acetate. The organic layer was dried and evaporated and the residue crystallized with ether/pet ether to give 2-dimethylamino-5-nitro-benzoic acid (1.14 g, 57%).

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureto reflux for 3 days
  3. extractionextracted with ethyl acetate
  4. customThe organic layer was dried
  5. customevaporated
  6. customthe residue crystallized with ether/pet ether