Ammonia → 2,5'-Bi-1H-benzimidazole, 1-methyl-2'-propyl-

HRID 1081891Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1081891
S(O)(O)(=O)=O.[CH2:6]([C:9]1[NH:10][C:11]2[CH:17]=[C:16]([C:18](O)=O)[CH:15]=[CH:14][C:12]=2[N:13]=1)[CH2:7][CH3:8].C([C:24]1[NH:25][C:26]2[CH:32]=[C:31](C(O)=O)[CH:30]=[CH:29][C:27]=2[N:28]=1)CC.Cl.Cl.CNC1C=CC=CC=1N.N>O>[CH2:6]([C:9]1[NH:10][C:11]2[CH:17]=[C:16]([C:18]3[N:25]([CH3:24])[C:26]4[CH:32]=[CH:31][CH:30]=[CH:29][C:27]=4[N:28]=3)[CH:15]=[CH:14][C:12]=2[N:13]=1)[CH2:7][CH3:8]

Komponenten

5

Edukt 3

HCID 222AmmoniaHCID 91296N-Methyl-o-phenylenediamine dihydrochlorideHCID 856442212-n-Propyl-benzimidazole-5-carboxylic acid-hemisulphate

Produkt 1

HCID 104694762,5'-Bi-1H-benzimidazole, 1-methyl-2'-propyl-

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A solution of 6.7 g (25 mMol) of 2-n-propyl-benzimidazole-5-carboxylic acid-hemisulphate and 4.9 g (25 mMol) of 2-methylaminoaniline-dihydrochloride in 200 g of polyphosphoric acid is stirred for 5 hours at 150° C., then poured onto 600 ml of water and made alkaline with concentrated ammonia whilst cooling with ice. The resulting solution is extracted three times with 200 ml of ethyl acetate, the crude product thus obtained is purified by column chromatography (300 g of silica gel; eluant:methylene chloride/methanol=15:1).

Aufarbeitung

  1. temperaturewhilst cooling with ice
  2. extractionThe resulting solution is extracted three times with 200 ml of ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-17489800f8014dd3a9fa3e6eb598427c
Quelldatensatz
uspto-grants-1996_12
Patentnummer
US05587393

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