HCID 21317692, Verbindung → Fluclotizolam

HRID 262976Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 262976
[C:1]([NH:4][NH:5][C:6]1[CH2:7][N:8]=[C:9]([C:17]2[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=2[F:23])[C:10]2[CH:15]=[C:14]([Cl:16])[S:13][C:11]=2[N:12]=1)(=O)[CH3:2]>C1(C)C(C)=CC=CC=1>[Cl:16][C:14]1[S:13][C:11]2[N:12]3[C:1]([CH3:2])=[N:4][N:5]=[C:6]3[CH2:7][N:8]=[C:9]([C:17]3[CH:22]=[CH:21][CH:20]=[CH:19][C:18]=3[F:23])[C:10]=2[CH:15]=1

Komponenten

3

Edukt 1

HCID 21317692HCID 21317692, Verbindung

Produkt 1

HCID 21317700Fluclotizolam

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 7237O-XyleneLösungsmittel

Versuchsvorschrift

6.8 g of 2-(2-acetylhydrazino)-7-chloro-5-(o-fluorophenyl)-3H-thieno[2,3-e]-1,4-diazepine are refluxed for 9 hours in 300 ml of absolute xylene. After cooling, the precipitated impurities are filtered off under vacuum. The solvent is then evaporated under reduced pressure and the product recrystallized from ethyl acetate containing active carbon to yield 2-chloro-4-(o-fluorophenyl)-9-methyl-6H-thieno[3,2-f]-s-triazolo[4,3-a][1,4]diazepine, melting point 187°-189° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. filtrationthe precipitated impurities are filtered off under vacuum
  3. customThe solvent is then evaporated under reduced pressure
  4. customthe product recrystallized from ethyl acetate containing active carbon

Quellen und Nachweise

ORD-Eintrag
ord-705bf0a3a623430d9df117106fb0cbe8
Quelldatensatz
uspto-grants-1979_05
Patentnummer
US04155913

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