HRID1487191

反应详情

EQUATION

反应方程式

HRID 1487191 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a flask equipped with a Dean-Stark water separator, 5-chloro-2-nitrobenzaldehyde (12.0 g, 64.7 mmol), ethylene glycol (8.0 g, 129.3 mmol) and p-toluenesulfonic acid (0.2 g) were dissolved in toluene (150 mL). The mixture was stirred at reflux for 8 hours. Dichloromethane was added and the organic phase was washed with saturated sodium bicarbonate and brine, then dried over anhydrous sodium sulfate, evaporated and purified by silica gel chromatography to afford the product 2-(5-chloro-2-nitrophenyl)-1,3-dioxolane (13.4 g, yield 90.0%).

WORKUP

后处理

  1. temperatureat reflux for 8 hours
  2. washthe organic phase was washed with saturated sodium bicarbonate and brine
  3. dry with materialdried over anhydrous sodium sulfate
  4. customevaporated
  5. custompurified by silica gel chromatography