反应 #640520

ord-18f14deab7bd4f55833e5a6152a7b1fa

反应方程式

N#CCCNc1nonc1-c1nc2ccccc2[nH]1
4-(1H-benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=C(CBr)c1ccc(Cl)cc1
4-chlorophenacyl bromide
N#CCCNc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)cc1
title compound
N#CCCNc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)cc1
4-[1-(4-Chlorophenacyl)-1H-benzimidazol-2-yl]-furazan-3-yl-N-(2-cyanoethyl)-amine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    洗涤washed with water
  2. 2
    干燥dried over sodium sulphate
  3. 3
    过滤Filtration of the sodium sulphate, concentration of the filtrate under reduced pressure and chromatography of the residue on silicagel

实验过程

A suspension of 4-(1H-benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine (0.10 g, 0.39 mmol), potassium carbonate (0.08 g, 0.58 mmol) and 4-chlorophenacyl bromide (0.11 g, 0.47 mmol) in DMF (5 ml) is stirred at room temperature for 16 hours. The reaction mixture is diluted with ethyl acetate, washed with water and dried over sodium sulphate. Filtration of the sodium sulphate, concentration of the filtrate under reduced pressure and chromatography of the residue on silicagel using hexane-ethyl acetate as eluent gives the title compound as a yellowish solid, m.p. 191-192° C.

来源

DOI: 10.6084/m9.figshare.5104873.v1专利: USRE042890E1uspto-grants-2011_11