HRID3710

反应详情

EQUATION

反应方程式

HRID 3710 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
23 °C

PROCEDURE

实验过程

A solution of 2,2'-dithiobisbenzoyl chloride (1.20 g, 3.50 mmol) in 25 mL of dichloromethane was added to a solution of 4-tert-butylaniline (1.04 g, 6.99 mmol) in 8 mL of pyridine at 23° C. The reaction mixture was stirred for 18 hours at 23° C. under nitrogen atmosphere. The mixture was concentrated, the residue triturated with 5% aqueous HCl, and the resulting solid was collected by filtration and washed with water to yield the crude product. The crude material was recrystallized from ethyl ether-ethanol to yield 0.24 g of the title compound, mp 135°-138° C.

WORKUP

后处理

  1. concentrationThe mixture was concentrated
  2. customthe residue triturated with 5% aqueous HCl
  3. filtrationthe resulting solid was collected by filtration
  4. washwashed with water
  5. customto yield the crude product
  6. customThe crude material was recrystallized from ethyl ether-ethanol