HRID1657028

反应详情

EQUATION

反应方程式

HRID 1657028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a mixture of S,N-dimethyl-N'-nitroisothiourea (0.5 g), CH3CN (20 ml) and potassium carbonate (0.93 g) was added a solution of phenylacetyl chloride (1.04 g) in CH3CN (2 ml) dropwise at room temperature over 10 minutes under stirring. After stirring for 3 hours, insolubles were filtered off and the filtrate was concentrated in vacuo. The resulting residue was applied to column chromatography on silica gel. The column was eluted with hexaneacetone (2:1) to afford 0.54 g of S,N-dimethyl-N'-nitro-N-phenylacetylisothiourea as an oil.

WORKUP

后处理

  1. stirringAfter stirring for 3 hours
  2. filtrationinsolubles were filtered off
  3. concentrationthe filtrate was concentrated in vacuo
  4. washThe column was eluted with hexaneacetone (2:1)