HRID1471024

反应详情

EQUATION

反应方程式

HRID 1471024 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a mixture of zinc chloride (39.1 g, 287 mmol) in benzene (215 mL) was added diethylamine (22.24 mL, 215 mmol) and 2-methylpropan-2-ol (20.57 mL, 215 mmol). The resulting mixture was stirred at rt for 2 h, and 2-bromo-1-(4-nitrophenyl)ethanone (35.0 g, 143 mmol) and 1-(4-chloro-3-nitrophenyl)ethanone (42.9 g, 215 mmol) were added in one portion. The resulting mixture was stirred at rt overnight. Added 5% aq. H2SO4 (50 mL) and stirred vigorously to induce precipitation. The resulting solid was collected by filtration and washed successively with benzene, water, methanol, and CH2Cl2. The solid was dried in vacuo to give the title compound.

WORKUP

后处理

  1. stirringThe resulting mixture was stirred at rt overnight
  2. stirringstirred vigorously
  3. customprecipitation
  4. filtrationThe resulting solid was collected by filtration
  5. washwashed successively with benzene, water, methanol, and CH2Cl2
  6. customThe solid was dried in vacuo