Diazomethane → HCID 20449998, Verbindung

HRID 358063Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 358063
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:12](=[O:15])[NH:13][N:14]=[C:10]3[CH2:9][CH:8]=[C:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[F:22])[C:6]=2[CH:23]=1.[N+](=[CH2:26])=[N-]>CO.C(Cl)Cl>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]3[C:12](=[O:15])[N:13]([CH3:26])[N:14]=[C:10]3[CH2:9][CH:8]=[C:7]([C:16]3[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=3[F:22])[C:6]=2[CH:23]=1

Komponenten

5

Edukt 2

HCID 9550Diazomethane2×HCID 20450024HCID 20450024, Verbindung

Produkt 1

HCID 20449998HCID 20449998, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittelHCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

A solution of 2.65 g of 8-chloro-6-(2-fluorophenyl)-2,4-dihydro-1H-s-triazolo[4,3-a][1]benzazepin-1-one in a mixture of 16 ml of methanol and 16 ml of methylene chloride is treated at 0° with 100 ml of ethereal diazomethane solution. After 3 hours, a further 33 ml of diazomethane solution are added and the mixture is left to stand for a further 2 hours. After evaporation of the solution, the residue is chromatographed on 80 g of silica gel while eluting with chloroform/ethanol (99:1). The crude product is recrystallized from ether/hexane. There is obtained 8-chloro-6-(2-fluorophenyl)-2,4-dihydro-2-methyl-1H-s-triazolo[4,3-a][1]benzazepin-1-one of melting point 142°-143°.

Aufarbeitung

  1. waitthe mixture is left
  2. waitto stand for a further 2 hours
  3. customAfter evaporation of the solution
  4. customthe residue is chromatographed on 80 g of silica gel
  5. washwhile eluting with chloroform/ethanol (99:1)
  6. customThe crude product is recrystallized from ether/hexane

Quellen und Nachweise

ORD-Eintrag
ord-a1b93e1922c34918bcf34f53d4b2277d
Quelldatensatz
uspto-grants-1984_08
Patentnummer
US04464300

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