반응 #640525

ord-5f20e0787c0e4fac869aed3bd63a8442

반응 방정식

N#CCCNc1nonc1-c1nc2ccccc2[nH]1
4-(1H-benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine
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
ICI
diiodomethane
Cc1ccc(O)cc1C
3,4-dimethylphenol
Cc1ccc(OCn2c(-c3nonc3NCCC#N)nc3ccccc32)cc1C
title compound
Cc1ccc(OCn2c(-c3nonc3NCCC#N)nc3ccccc32)cc1C
4-[1-(3,4-Dimethylphenoxymethyl)-1H-benzimidazol-2-yl]-furazan-3-yl-N-(2-cyanoethyl)-amine

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    세척washed with water
  2. 2
    건조dried over sodium sulphate
  3. 3
    여과Filtration of the sodium sulphate, concentration of the filtrate under reduced pressure and chromatography of the residue on silicagel

실험 절차

A suspension of 4-(1H-benzimidazol-2-yl)-furazan-3-yl-N-(2-cyanoethyl)-amine (0.15 g, 0.59 mmol, Example 6a), potassium carbonate (0.325 g, 2.36 mmol), diiodomethane (0.16 g, 0.59 mmol) and 3,4-dimethylphenol (0.072 g, 0.59 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. 132-135° C.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: USRE042890E1uspto-grants-2011_11