HRID1973402

反应详情

EQUATION

反应方程式

HRID 1973402 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

A mixture of 34.8 g (0.22 mol) of gramine and 23.9 g (0.20 mol) of nitrosopiperazine in 700 ml. of toluene is refluxed while stirring under nitrogen for 48 hours. The reaction solution is then concentrated under reduced pressure until a precipitate appears and then is cooled to 0° C. and is filtered. The product is washed with cold toluene and dried to produce crystals of 3-(4-nitrosopiperazin-1-yl)methylindole. This product is recrystallized from toluene to yield pure plates, m.p. 116°-118° C. Analysis: Calculated for C13H16N4O: 63.92% C; 6.60% H; 22.93% N Found: 63.84% C; 6.64% H; 23.06% N.

WORKUP

后处理

  1. concentrationThe reaction solution is then concentrated under reduced pressure until a precipitate
  2. filtrationis filtered
  3. washThe product is washed with cold toluene
  4. customdried