Water → HCID 178441464, Verbindung

HRID 1655476Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1655476
[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:16]=[CH:15][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]#[N:24])=[CH:13][CH:12]=2)[C:8]2[C:25]([CH2:29][OH:30])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4].[N-:31]=[N+:32]=[N-:33].[Na+].[Cl-].[NH4+].O>CN(C=O)C>[CH2:1]([C:5]1[N:9]([CH2:10][C:11]2[CH:12]=[CH:13][C:14]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[C:23]3[NH:33][N:32]=[N:31][N:24]=3)=[CH:15][CH:16]=2)[C:8]2[C:25]([CH2:29][OH:30])=[CH:26][CH:27]=[CH:28][C:7]=2[N:6]=1)[CH2:2][CH2:3][CH3:4]

Komponenten

6

Edukt 4

HCID 962WaterHCID 25517Ammonium ChlorideHCID 33557Sodium AzideHCID 19792172HCID 19792172, Verbindung

Produkt 1

HCID 178441464HCID 178441464, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
115 °C

Versuchsvorschrift

A mixture of 2-butyl-1-[(2'-cyanobiphenyl-4-yl)methyl]-7-hydroxymethylbenzimidazole (0.4 g), sodium azide (0.98 g) and ammonium chloride (0.8 g) in DMF (4 ml) was stirred for 4 days at 110-120° C. To the reaction mixture was added water, which was extracted with ethyl acetate. The extract was washed with water and dried. After removal of the solvent, the residue was crystallized from ethyl acetate-methanol to give colorless needles, m.p. 152-153° C.

Aufarbeitung

  1. extractionwas extracted with ethyl acetate
  2. washThe extract was washed with water
  3. customdried
  4. customAfter removal of the solvent
  5. customthe residue was crystallized from ethyl acetate-methanol
  6. customto give colorless needles, m.p. 152-153° C.

Quellen und Nachweise

ORD-Eintrag
ord-be169c623d7b4f898e817ff1903dfbb4
Quelldatensatz
uspto-grants-1993_10
Patentnummer
US05250554

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