HRID2203116

反应详情

EQUATION

反应方程式

HRID 2203116 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 2,2-diethoxyethanethioamide (2 g), ethyl bromopyruvate (1.61 ml), MS-4A (2 g) and EtOH (15 ml) was heated under reflux for 1 h. The mixture was concentrated, and the residue was diluted with AcOEt. The mixture was washed with water and brine successively, dried with MgSO4 and concentrated in vacuo. The residue was purified by NH silica gel column chromatography (hexane/EtOAc) to give the title compound (2.5 g) as an off-white solid.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureunder reflux for 1 h
  3. concentrationThe mixture was concentrated
  4. additionthe residue was diluted with AcOEt
  5. washThe mixture was washed with water and brine successively
  6. dry with materialdried with MgSO4
  7. concentrationconcentrated in vacuo
  8. customThe residue was purified by NH silica gel column chromatography (hexane/EtOAc)