HRID2232044

反应详情

EQUATION

反应方程式

HRID 2232044 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
22 °C

PROCEDURE

实验过程

Into a 500 mL flask was placed 300 mL of distilled methylene chloride (distilled from P2O5) and 5.0 g (16 mmol) of commercial diphenyliodonium chloride (Aldrich Chemical Co.). The heterogeneous mixture was stirred vigorously in a water bath at 22° C. and 3.19 ml (3.91 g, 17.6 mmol) of trimethylsilyl triflate was added. The solid dissolved almost immediately but a precipitate reappeared after 5 m. The reaction was stirred for 15 h and the solvent removed on the rotary evaporator. The residue was triturated with ether to yield 6.5 g (96%) of the iodonium triflate 1 (mp 165°-8° C.). The material tested negative for chloride with silver nitrate-ethanol. The aryl iodonium triflates 3 and 4 were produced in a similar fashion.

WORKUP

后处理

  1. customInto a 500 mL flask was placed
  2. dissolutionThe solid dissolved almost immediately
  3. stirringThe reaction was stirred for 15 h
  4. customthe solvent removed on the rotary evaporator
  5. customThe residue was triturated with ether