HRID487195

反应详情

EQUATION

反应方程式

HRID 487195 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a stirred solution of 3-nitro-2,5,6-trichlorobenzoic acid (37.1 mmol, 10.0 g) in 150 mL of toluene, was added 2-chlorobenzylamine (81.6 mmol, 11.56 g). The reaction mixture was refluxed overnight, poured into dilute hydrochloric acid and vigorously stirred. The resulting solid was filtered. The product was dissolved in toluene and then precipitated with diethyl ether. Recrystallization of the product from methanol gave 3.4 g of 2-[2-chlorophenyl)methyl]amino-5,6-dichloro-3-nitrobenzoic acid; mp 168.5°-171° C.

WORKUP

后处理

  1. temperatureThe reaction mixture was refluxed overnight
  2. filtrationThe resulting solid was filtered
  3. dissolutionThe product was dissolved in toluene
  4. customprecipitated with diethyl ether
  5. customRecrystallization of the product from methanol