HRID4139

反应详情

EQUATION

反应方程式

HRID 4139 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2-ethylbenzenesulfonyl chloride (obtained by chlorosulfonation of ethylbenzene) (7.78 g) in carbon tetrachloride (5.0 ml) was contacted with a solution of dichlorine monoxide (82 mmol) in carbon tetrachloride (100 ml) and the mixture was heated in a closed system at 50°-60° for 16 hrs. The mixture was dried (MgSO4) and volatiles were removed under vacuum. The residue was kugelrohr distilled to give 7.63 g of colorless oil, bp 75°-80° (0.15 mm). 1H nmr δCDCl3TMS 8.20-7.35 (m). 6.13 (q, J=7 Hz), 1.90 (d, J=7 Hz).

WORKUP

后处理

  1. temperaturethe mixture was heated in a closed system at 50°-60° for 16 hrs
  2. dry with materialThe mixture was dried (MgSO4) and volatiles
  3. customwere removed under vacuum
  4. distillationThe residue was kugelrohr distilled