HRID488520

反应详情

EQUATION

反应方程式

HRID 488520 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A mixture of o-bromobenzoic acid potassium salt (47.8 g, 0.2 mol), 4-iodoaniline (43.8 g, 0.2 mol), K2CO3 (13.8 g, 0.1 mol), and cupric acetate (2.87 g, 6%) in diglyme (100 mL) was heated to reflux for 30 minutes. The reaction mixture was diluted with H2O (1.0 L) and filtered. The filtrate was acidified with diluted AcOH. The resulting precipitate was collected by filtration, washed with H2O and dried in a vacuum at 50° C. for 16 hours. Recrystallization from EtOAc gave the desired product, a solid (29.7 g, 0.087 mol, 44%). mp 205-206° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux for 30 minutes
  3. filtrationfiltered
  4. filtrationThe resulting precipitate was collected by filtration
  5. washwashed with H2O
  6. customdried in a vacuum at 50° C. for 16 hours
  7. customRecrystallization from EtOAc