反应 #452464

ord-7db9d80f2df64dc6835abcda7aa64ffe

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    温度heated
  2. 2
    温度at reflux for 4 h
  3. 3
    其他The solvent was removed by evaporation in vacuo
  4. 4
    其他the residue (3.09 g) purified by column chromatography on silica gel (400 ml)

实验过程

N-(4-bromobenzyl)-N-(3-isothiocyanatopropyl)-N-(pyridin-2-yl)amine(1 g, 2.76 mmol) and 3-(1-triphenylmethylimidazol-4-yl)propylamine (1.014 g, 2.76 mmol) were dissolved in chloroform (10 ml) and heated at reflux for 4 h. The solvent was removed by evaporation in vacuo and the residue (3.09 g) purified by column chromatography on silica gel (400 ml) using ethyl acetate/methanol/triethylamine 9:0.5:0.5 as eluent affording 1.59 g (80%) of pure 1-[3-(1-triphenylmethylimidazol-4-yl)propyl]-3-[3-[N-(4-bromobenzyl)-N-(pyridin-2-yl)amino]propyl]thiourea.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: US06127343uspto-grants-2000_10