Ammonia → 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide

HRID 67485Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 67485
[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([O:19]CC)=O)=[C:4]2[CH2:3]1.[Cl-].[NH4+:23].N>CO>[CH3:1][N:2]1[C:8](=[O:9])[C:7]2[CH:10]=[CH:11][CH:12]=[CH:13][C:6]=2[N:5]2[CH:14]=[N:15][C:16]([C:17]([NH2:23])=[O:19])=[C:4]2[CH2:3]1

Komponenten

5

Edukt 3

HCID 222AmmoniaHCID 25517Ammonium ChlorideHCID 127597Ro 14-7437

Produkt 1

HCID 205153215,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A mixture of 10.0 g of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate, 200 ml of methanol, 0.5 g of ammonium chloride and 30 g of ammonia (100%) is stirred in an autoclave under nitrogen (40 bar) at a temperature of 120° C. for 12 hours. After cooling and discharging the over-pressure, the mixture is evaporated to dryness. After partition of the residue between methylene chloride and water, the organic phase is dried and evaporated. The residue is recrystallised from ethyl acetate, there being obtained 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxamide in the form of white crystals of melting point 274°-275° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. customthe mixture is evaporated to dryness
  3. customAfter partition of the residue between methylene chloride and water
  4. customthe organic phase is dried
  5. customevaporated
  6. customThe residue is recrystallised from ethyl acetate, there

Quellen und Nachweise

ORD-Eintrag
ord-ea97190421b9439d8396e8017932bcd9
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346034

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