HRID1732607
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
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
- filtrationThe mixture was filtered
- customto give a yellow solid
- customthe aqueous phase of the filtrate was separated
- extractionextracted with ether (2×150 ml)
- customThe combined ether solutions were evaporated to a residue
- filtrationThis residue and the solid filtered off
- customearlier were recrystallised from acetone-chloroform