HRID2101230

反应详情

EQUATION

反应方程式

HRID 2101230 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

4′-Fluoro-biphenyl (0.03 mol) was added to 1 M AlCl3 in nitrobenzene (40 mL, 0.04 mol) with chilling in an ice bath. Acetyl chloride (0.06 mol) was added dropwise and the mixture stirred overnight at room temperature. The dark solution was poured into a mixture of crushed ice (150 mL), water (25 mL) and HCl (50 mL). The aqueous phase was separated and the nitrobenzene removed by steam distillation to give a dark low melting solid. The solid was recrystallised from aqueous methanol to give the title compound. δC (CDCl3, 62.9 MHz): 26.7, 115.9 (d, J 21.5), 127.1, 129.0 (d, J=7.8), 135.8, 136.0 (d, J 2.9), 144.7, 163.0 (d, J 248.0) and 197.8.

WORKUP

后处理

  1. temperaturewith chilling in an ice bath
  2. customThe aqueous phase was separated
  3. customthe nitrobenzene removed by steam distillation
  4. customto give a dark low melting solid
  5. customThe solid was recrystallised from aqueous methanol