反应 #640523

ord-c0321566886c4792b918bc68f9089675

反应方程式

ICI
diiodomethane
Nc1nonc1-c1nc2ccccc2[nH]1
4-(1H-benzimidazol-2-yl)-furazan-3-ylamine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
Oc1ccc(F)cc1
4-fluorophenol
Nc1nonc1-c1nc2ccccc2n1COc1ccc(F)cc1
title compound
Nc1nonc1-c1nc2ccccc2n1COc1ccc(F)cc1
4-[1-(4-Fluorophenoxymethyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine

反应条件

详细条件
See reaction.notes.procedure_details.

后处理

  1. 1
    其他Evaporation of the solvent under reduced pressure
  2. 2
    其他partitioning of the resulting residue between water and ethyl acetate
  3. 3
    干燥by drying of the organic solution over sodium sulphate and chromatography of the residue

实验过程

To a solution of 4-(1H-benzimidazol-2-yl)-furazan-3-ylamine (0.10 g, 0.497 mmol) is added potassium carbonate (0.172 g, 1.24 mmol) followed by 4-fluorophenol (0.0557 g, 0.497 mmol) and diiodomethane (0.133 g, 0.497 mmol). The mixture is stirred over night. Evaporation of the solvent under reduced pressure and partitioning of the resulting residue between water and ethyl acetate followed by drying of the organic solution over sodium sulphate and chromatography of the residue gives the title compound as a colorless solid, m.p. 155-158° C.

来源

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