HRID256178

反应详情

EQUATION

反应方程式

HRID 256178 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Prepared as described by D. E. O'Brien et al, J. Het. Chem., 7, 102 (1970) as follows. A mixture of 5-chloro-2-nitrobenzaldehyde (18.3 g, 0.1 mole), ethylene glycol (7.0 g, 0.11 mole) p-toluenesulfonic acid (0.5 g) and benzene (850 mL) was stirred and refluxed with continuous removal of water via a Dean and Stark trap for 24 hours. The solvent was removed, the residue dissolved in dichloromethane and filtered through a plug of silica gel (6" deep). Evaporation of the solvent afforded 2-(5-chloro-2-nitrophenyl)-1,3-dioxolane (21.8 g, 97%) as an oil.

WORKUP

后处理

  1. customPrepared
  2. customThe solvent was removed
  3. dissolutionthe residue dissolved in dichloromethane
  4. filtrationfiltered through a plug of silica gel (6" deep)
  5. customEvaporation of the solvent