Potassium Cyanide → isopropyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine 3-carboxylate

HRID 67321Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 67321
[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][CH2:20][CH3:21])=[O:18])=[C:4]2[CH2:3]1.[C-:22]#N.[K+]>CC(O)C>[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][CH:20]([CH3:22])[CH3:21])=[O:18])=[C:4]2[CH2:3]1

Komponenten

4

Edukt 2

HCID 9032Potassium CyanideHCID 127597Ro 14-7437

Produkt 1

HCID 19735056isopropyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine 3-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 3776IsopropanolLösungsmittel

Versuchsvorschrift

285 mg (1 mmol) of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate and 50 mg of potassium cyanide are stirred at 60° C. for 72 hours in 10 ml of 2-propanol. Then, the mixture is concentrated on a rotary evaporator, the residue is partitioned between water and chloroform, extracted twice with chloroform, the chloroform phase is dried over magnesium sulphate and evaporated. There is obtained isopropyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine 3-carboxylate of melting point 190°-192° C. This product is uniform according to thin-layer chromatography.

Aufarbeitung

  1. concentrationThen, the mixture is concentrated on a rotary evaporator
  2. customthe residue is partitioned between water and chloroform
  3. extractionextracted twice with chloroform
  4. dry with materialthe chloroform phase is dried over magnesium sulphate
  5. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-5900985991ac45158a44abf67892676c
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346030

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