HRID2203116
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperaturewas heated
- temperatureunder reflux for 1 h
- concentrationThe mixture was concentrated
- additionthe residue was diluted with AcOEt
- washThe mixture was washed with water and brine successively
- dry with materialdried with MgSO4
- concentrationconcentrated in vacuo
- customThe residue was purified by NH silica gel column chromatography (hexane/EtOAc)