HRID988900

反应详情

EQUATION

反应方程式

HRID 988900 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
45 °C

PROCEDURE

实验过程

To a solution of 4-chloro-2-iodoaniline (16.5 g, 65.1 mmol) in DMF (250 mL) at rt were added a-bromodiphenylmethane (21.5 g, 84.6 mmol) and iPr2NEt (23 mL, 130 mmol) and the reaction mixture was heated at 45° C. overnight. After the volatile was removed under reduced pressure, the residue was dissolved in EtOAc, washed with water (3x) and brine and dried over MgSO4. Purification on SiO2 column chromoatography (hexanes to 5% EtOAc/hexanes) gave the desired Benzhydryl-(4-chloro-2-iodo-phenyl)-amine (26.1 g, 97% yield) as a yellowish solid.

WORKUP

后处理

  1. customAfter the volatile was removed under reduced pressure
  2. dissolutionthe residue was dissolved in EtOAc
  3. washwashed with water (3x) and brine
  4. dry with materialdried over MgSO4
  5. customPurification on SiO2 column chromoatography (hexanes to 5% EtOAc/hexanes)