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Ammonia → HCID 20393008, Verbindung

HRID 1862989
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1862989
[NH2:1][C:2]1[CH:7]=[C:6]([O:8][CH:9]([CH3:11])[CH3:10])[C:5]([O:12][CH:13]([CH3:15])[CH3:14])=[CH:4][C:3]=1[NH2:16].[N:17]#[C:18]Br.N.C(Cl)(Cl)Cl>CO.O>[NH2:17][C:18]1[NH:16][C:3]2[CH:4]=[C:5]([O:12][CH:13]([CH3:15])[CH3:14])[C:6]([O:8][CH:9]([CH3:11])[CH3:10])=[CH:7][C:2]=2[N:1]=1
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Komponenten

7

Edukt 4

HCID 222AmmoniaHCID 6212ChloroformHCID 10476Cyanogen BromideHCID 132301804,5-Bis[(propan-2-yl)oxy]benzene-1,2-diamine

Produkt 1

HCID 20393008HCID 20393008, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel
HCID 962
Water
Lösungsmittel
2×

Versuchsvorschrift

A solution of 1,2-diamino-4,5-di-isopropoxybenzene (2.24 g.) in methanol (40 ml.) was added to a mixture of cyanogen bromide (1.6 g.) in water (40 ml.). The mixture was stirred at 20°-25° C. for 70 hours and then basified by addition of an excess of aqueous ammonia solution (density 0.88). The mixture was then separated by filtration and the filtrate evaporated. The residue which was obtained was mixed with water (50 ml.) and chloroform (50 ml.). The chloroform phase was separated, dried (MgSO4) and evaporated. The residual gum obtained, was purified by chromatography on a column of silica gel (40 g.) using methanol-chloroform (1:3 v/v) as eluant, to give 2-amino-5,6-di-isopropoxybenzimidazole as a sticky solid (1.2 g.), having characteristic absorption bands at ν 3400, 3320, 3080, 1660 and 1565 cm-1, in the infra-red (IR) spectrum.

Aufarbeitung

  1. customThe mixture was then separated by filtration
  2. customthe filtrate evaporated
  3. customThe residue which was obtained
  4. customThe chloroform phase was separated
  5. dry with materialdried (MgSO4)
  6. customevaporated
  7. customThe residual gum obtained
  8. customwas purified by chromatography on a column of silica gel (40 g.)

Quellen und Nachweise

ORD-Eintrag
ord-74b706814d4e47a1a40de4a7bb6596e8
Quelldatensatz
uspto-grants-1979_09
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US04167569

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