HRID1732607

反应详情

EQUATION

反应方程式

HRID 1732607 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Dry hydrogen chloride was passed through a stirred solution of 1-nitro-2-methylthio-2-(2,2-diethoxyethylamino)-ethylene (9.7g, 0.04 mol) in dry ether (250 ml) at 5-10° for 3 hours. The resulting mixture was basified by pouring it into potassium carbonate solution (300 ml). The mixture was filtered to give a yellow solid, and the aqueous phase of the filtrate was separated and extracted with ether (2×150 ml). The combined ether solutions were evaporated to a residue. This residue and the solid filtered off earlier were recrystallised from acetone-chloroform to give 2-methylthio-3-nitropyrrole (3.4g, 54%) m.p. 212-213°.

WORKUP

后处理

  1. filtrationThe mixture was filtered
  2. customto give a yellow solid
  3. customthe aqueous phase of the filtrate was separated
  4. extractionextracted with ether (2×150 ml)
  5. customThe combined ether solutions were evaporated to a residue
  6. filtrationThis residue and the solid filtered off
  7. customearlier were recrystallised from acetone-chloroform