HRID647093

反应详情

EQUATION

反应方程式

HRID 647093 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

(a)(i) A solution of aminoacetaldehyde diethylacetal (8 g, 0.06 mol) and 1-nitro-2,2-bis-methylthioethylene (10 g, 0.06 mol) in ethanol (100 ml) was refluxed for 20 hours. The solvent was removed in vacuo. The residue was chromatographed on a silica gel column eluted with carbon tetrachloride/chloroform (7:3) and the product was crystallised from propan-2-ol to give 1-nitro-2-methylthio-2-(2,2-diethoxyethylamino)ethylene (8.7 g, 58%) m.p. 73°-73.5°.

WORKUP

后处理

  1. customThe solvent was removed in vacuo
  2. customThe residue was chromatographed on a silica gel column
  3. washeluted with carbon tetrachloride/chloroform (7:3)
  4. customthe product was crystallised from propan-2-ol