HRID1290491

反应详情

EQUATION

反应方程式

HRID 1290491 的结构方程式

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

An intimate mixture of piperazinone (4.2 g) and 4-chloropyridine hydrochloride (7.33 g) was stirred and heated at 200° C. for 10 minutes and allowed to cool. The product was purified by flash column chromatography and cluted with 1/9/0.1 v:v:v methanol/methylene chloride/0.88 S.G. aqueous ammonia. The solid thus obtained was recrystallised from ethanol to give 4-(4-pyridyl)piperazin-2-one (1.75 g); m.p. 268°-270° C.; NMR (d6DMSO) δ 8.2(3H,m); 6.8(12H,m); 3.85(2H,s); 3.52(2H,m); 3.31(2H,m); m/e 178(M+H)+.

WORKUP

后处理

  1. temperatureto cool
  2. customThe product was purified by flash column chromatography
  3. customThe solid thus obtained
  4. customwas recrystallised from ethanol