反応 #640532

ord-bc19d117a55c4630b18be9f3c39e2601

反応方程式

Nc1nonc1-c1nc2ccccc2[nH]1
4-(1H-benzimidazol-2-yl)-furazan-3-ylamine
O=C([O-])[O-].[K+].[K+]
potassium carbonate
O=C(CBr)c1ccc(Cl)c([N+](=O)[O-])c1
4-chloro-3-nitrophenacyl bromide
Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)c([N+](=O)[O-])c1
title compound
Nc1nonc1-c1nc2ccccc2n1CC(=O)c1ccc(Cl)c([N+](=O)[O-])c1
4-[1-(4-Chloro-3-nitrophenacyl)-1H-benzimidazol-2-yl]-furazan-3-ylamine

反応条件

詳細条件
See reaction.notes.procedure_details.

後処理

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

実験手順

A suspension of 4-(1H-benzimidazol-2-yl)-furazan-3-ylamine (0.228 g, 1.14 mmol), potassium carbonate (0.40 g, 2.85 mmol) and 4-chloro-3-nitrophenacyl bromide (0.35 g, 1.25 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 solid, m.p. 198-200° C. (This compound is also listed as Example 66 in Table 1.)

出典

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