HRID1065759

反应详情

EQUATION

反应方程式

HRID 1065759 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Crushed potassium hydroxide (5.7 g, 0.1 mol) was added portionwise to a refluxing solution of 1-nitro-2-methylthio-2-methylsulphinylethylene (9.3 g, 0.05 mol) and aminoacetone hydrochloride (5.6 g, 0.05 mol) in methanol (100 ml). Reflux was continued for 5 minutes, and then the mixture was cooled and the solvent removed in vacuo. Water was added to the residue, and the solid was recrystallised from chloroform/methanol/petroleum ether to give 2-methylthio-3-nitro-4-methylpyrrole (1.45 g, 16%) m.p. 216-216-5.

WORKUP

后处理

  1. temperatureReflux
  2. temperaturethe mixture was cooled
  3. customthe solvent removed in vacuo
  4. additionWater was added to the residue
  5. customthe solid was recrystallised from chloroform/methanol/petroleum ether