反应 #52201

ord-1ccd850b8d5f4b728e33415745f93e9f

溶剂

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他The volatiles were removed by evaporation
  2. 2
    其他the residue was purified by chromatography
  3. 3
    洗涤eluting with hexane/dichloromethane (50:50)
  4. 4
    温度increasing in polarity to dichloromethane/methanol (80:20)

实验过程

1-(3-Aminopropyl)imidazole (2.39 ml, 0.02 mol) was added to a solution of 4-bromobenzoyl chloride (4.0 g, 0.218 mol) in ethanol (250 ml). The mixture was stirred at ambient temperature for 18 hours. The volatiles were removed by evaporation and the residue was purified by chromatography eluting with hexane/dichloromethane (50:50) increasing in polarity to dichloromethane/methanol (80:20) to give the title compound. NMR: 1.95 (m, 2H), 3.20 (q, 2H), 4.0 (t, 2H), 6.87 (s, 1H), 7.19 (s, 1H), 7.64 (d, 2H), 7.68 (s, 1H), 7.78 (d, 2H), 8.58 (t, 1H); m/z: 308 [MH]+.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06855719B1uspto-grants-2005_02