Flumazenil → isopropyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo [1,5-a][1,4]benzodiazepine-3-carboxylate

HRID 67292

Reaktionsgleichung

Reaktionsgleichung von HRID 67292
[H-].[Na+].[F:3][C:4]1[CH:5]=[CH:6][C:7]2[N:13]3[CH:14]=[N:15][C:16]([C:17]([O:19][CH2:20][CH3:21])=[O:18])=[C:12]3[CH2:11][N:10]([CH3:22])[C:9](=[O:23])[C:8]=2[CH:24]=1.[CH3:25]C(O)C>>[F:3][C:4]1[CH:5]=[CH:6][C:7]2[N:13]3[CH:14]=[N:15][C:16]([C:17]([O:19][CH:20]([CH3:25])[CH3:21])=[O:18])=[C:12]3[CH2:11][N:10]([CH3:22])[C:9](=[O:23])[C:8]=2[CH:24]=1

Komponenten

4

Edukt 3

HCID 3373FlumazenilHCID 3776IsopropanolHCID 24758Sodium hydride

Produkt 1

HCID 20515336isopropyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo [1,5-a][1,4]benzodiazepine-3-carboxylate

Versuchsvorschrift

100 ml of 2-propanol are treated with 100 mg of sodium hydride. 5 g of ethyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate are added thereto and the mixture is heated to boiling under reflux for 1 hour. Subsequently, the mixture is left to cool to room temperature, the separated crystals are filtered off and washed with 2-propanol and water, there being obtained isopropyl 8-fluoro-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 243°-244° C.

Aufarbeitung

  1. temperaturethe mixture is heated
  2. temperatureunder reflux for 1 hour
  3. waitSubsequently, the mixture is left
  4. filtrationthe separated crystals are filtered off
  5. washwashed with 2-propanol and water, there

Quellen und Nachweise

ORD-Eintrag
ord-f9bd880d0f834809bd9dbe54894d5a99
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346030

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