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Methane → HCID 178508147, Verbindung

HRID 1762117
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1762117
[NH2:1][C:2]1[C:16]([NH2:17])=[CH:15][C:5]2[N:6]=[C:7]([C:9]3[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=3)[NH:8][C:4]=2[CH:3]=1.[N:18]#[C:19]Br.C>>[NH2:18][C:19]1[NH:17][C:16]2[CH:15]=[C:5]3[N:6]=[C:7]([C:9]4[CH:14]=[CH:13][N:12]=[CH:11][CH:10]=4)[NH:8][C:4]3=[CH:3][C:2]=2[N:1]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 3

HCID 297MethaneHCID 10476Cyanogen BromideHCID 200424525,6-Diamino-2-(4-pyridyl)-benzimidazole

Produkt 1

HCID 178508147HCID 178508147, Verbindung

Versuchsvorschrift

2.9 g. 5,6-diamino-2-(4-pyridyl)-benzimidazole and 1.3 g. cyanogen bromide are stirred for 2 hours at 85° C. with the exclusion of moisture. After cooling to ambient temperature, the reaction mixture is treated with active charcoal, filtered and the filtrate evaporated to dryness. The residue is suspended in water, the pH value is adjusted to 8.5 with aqueous ammonia solution and filtered off with suction. The 1.47 g. of residue obtained is applied to 15 g. silica gel 60 and eluted with a mixture of methylene chloride and ammoniacal methanol (95:5 v/v to 92:8 v/v). The appropriate fractions are evaporated to dryness and the residue is dissolved in methanol. Isopropanol is added thereto until turbid and then left to crystallise. There is obtained 0.52 g. of the desired compound; m.p. >320° C.

Aufarbeitung

  1. filtrationfiltered
  2. customthe filtrate evaporated to dryness
  3. filtrationfiltered off with suction
  4. customof residue obtained
  5. washsilica gel 60 and eluted with a mixture of methylene chloride and ammoniacal methanol (95:5 v/v to 92:8 v/v)
  6. customThe appropriate fractions are evaporated to dryness
  7. dissolutionthe residue is dissolved in methanol
  8. additionIsopropanol is added
  9. waituntil turbid and then left
  10. customto crystallise
  11. customThere is obtained 0.52 g

Quellen und Nachweise

ORD-Eintrag
ord-2cabc4bcf61e4d3eb79df003f3a442fb
Quelldatensatz
uspto-grants-1989_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04831032

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