HRID2057804

反应详情

EQUATION

反应方程式

HRID 2057804 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 0.4 moles sodium in absolute dimethylformamide is saturated by passing in hydrogen sulfide for 5 hours. There is then added in portions 0.05 moles of 2-methyl-3-ethoxycarbonyloxy-4-ethoxycarbonyloxymethyl-5-chloromethylpyridine and the mixture stirred overnight at room temperature with hydrogen sulfide slowly bubbling through the mixture. The reaction mixture is then concentrated in vacuo and taken up between ethyl acetate and water containing acetic acid. The ethyl acetate layer is removed, dried over sodium sulfate and concentrated to give 2-methyl-3-ethoxycarbonyloxy-4-ethoxycarbonyloxymethyl-5-mercaptomethylpyridine.

WORKUP

后处理

  1. customslowly bubbling through the mixture
  2. concentrationThe reaction mixture is then concentrated in vacuo
  3. additioncontaining acetic acid
  4. customThe ethyl acetate layer is removed
  5. dry with materialdried over sodium sulfate
  6. concentrationconcentrated