HRID988873

反应详情

EQUATION

反应方程式

HRID 988873 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 α-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 (3×) 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 (3×) and brine
  4. dry with materialdried over MgSO4
  5. customPurification on SiO2 column chromoatography (hexanes to 5% EtOAc/hexanes)