HRID614938

反应详情

EQUATION

反应方程式

HRID 614938 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Hydrogen chloride gas was introduced into a mixture of 2-acetoxyethanethiol (24.0 g) and paraformaldehyde (6.0 g) at a moderate rate with external cooling for 3 hours. Calcium chloride (25 g) was added and the reaction mixture allowed to stand in a salt-ice bath for 4 hours. Methylene chloride (200 ml) was added, the reaction mixture filtered and the solvent evaporated with rigorous exclusion of moisture. The residual oil was distilled to give 2-acetyloxyethyl chloromethyl sulfide (18.5 g, bp 82°-87° C. at 3 mm Hg).

WORKUP

后处理

  1. temperaturewith external cooling for 3 hours
  2. filtrationthe reaction mixture filtered
  3. customthe solvent evaporated with rigorous exclusion of moisture
  4. distillationThe residual oil was distilled