反应 #1687662

反应方程式

2,5-dibromo piperazine

piperazine

potassium carbonate

→

(5-bromopyridin-2-yl)-piperazine

溶剂

acetonitrile

反应条件

后处理

1. 1
   温度at reflux for 48 h
2. 2
   过滤The solid was filtered off
3. 3
   洗涤washed with acetonitrile (50 mL)
4. 4
   浓缩The organics were concentrated to a tan solid
5. 5
   其他The product was purified by column chromatography on silica gel

实验过程

A solution of 2,5-dibromo piperazine (1.59 g, 8 mmole), and piperazine(1.45 g, 16 mmole), and potassium carbonate (6 g) in acetonitrile (50 mL) was heated at reflux for 48 h. The heating was discontinued and the solution allowed to cool to room temperature. The solid was filtered off and washed with acetonitrile (50 mL). The organics were concentrated to a tan solid. The product was purified by column chromatography on silica gel using dichloromethane:methanol:triethylamine (94:5:1) as eluent to provide (5-bromopyridin-2-yl)-piperazine as an offwhite solid (1.75 g, 95%). δH (300 MHz CDCl3) 1.75 (1H, br s), 2.95 (4H, m, piperaziny), 3.45 (4H, m, piperazinyl), 6.52 (1H, d, J=9.0), 7.51 (1H, dd, J=2.5 and 9.0), 8.17 (1H, d, J=2.4), ESMS 243 (MH+).

来源