HRID404531

反应详情

EQUATION

反应方程式

HRID 404531 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A stirred mixture of triphenylacetic acid (21.7 g; 0.075 mol) and dry dimethylformamide (2 drops) in dry dichloromethane (100 cm3) was treated with oxalyl chloride (14 g; 0.11 mol) which was added in 4 approximately equal portions over ˜25 minutes. The mixture was stirred at 35° until evolution of hydrogen chloride had ceased (˜4 hrs). The resulting colourless solution was evaporated in vacuo at 40° to constant weight to give the title compound as a colourless crystalline solid. Yield=23.24 g (100.0%). The product was used directly in next stage.

WORKUP

后处理

  1. additionwas added in 4 approximately equal portions over ˜25 minutes
  2. custom(˜4 hrs)
  3. customThe resulting colourless solution was evaporated in vacuo at 40° to constant weight