反应 #312610

ord-acb0fdec938349bfba9edaea14747266

反应方程式

Brc1cccc2nc[nH]c12
4-bromobenzimidazole
C1CNCCNC1
homopiperazine
CC(C)(C)[O-].[Na+]
NaOt-Bu
c1cc(N2CCCNCC2)c2[nH]cnc2c1
4-(homopiperazin-1-yl)benzimidazole

反应条件

温度
120°CELSIUS
详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度cooled to room temperature
  2. 2
    萃取The aqueous mixture is extracted with ethyl acetate
  3. 3
    干燥dried over MgSO4
  4. 4
    浓缩concentrated in vacuo
  5. 5
    其他to give a residue
  6. 6
    其他The residue is purified by flash chromatography

实验过程

A suspension of 4-bromobenzimidazole (42 mmol), homopiperazine (256 mmol) and NaOt-Bu (59 mmol) in dry o-xylene, under N2, is treated with a catalytic amount of Pd (OCOCH3)2·P(t-Bu)3 (P/Pd=4), heated at 120° C. for 3 hr, cooled to room temperature and diluted with water. The aqueous mixture is extracted with ethyl acetate. The extracts are combined, dried over MgSO4 and concentrated in vacuo to give a residue. The residue is purified by flash chromatography to give 4-(homopiperazin-1-yl)benzimidazole.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US07557098B2uspto-grants-2009_07