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

HRID 67320

Reaktionsgleichung

Reaktionsgleichung von HRID 67320
[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]C)=[O:18])=[C:4]2[CH2:3]1.[C-]#N.[K+]>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]([O:19][CH3:20])=[O:18])=[C:4]2[CH2:3]1

Komponenten

4

Edukt 2

HCID 9032Potassium CyanideHCID 127597Ro 14-7437

Produkt 1

HCID 10378479methyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

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 66 mg of potassium cyanide are heated to boiling under reflux for 24 hours in 10 ml of methanol. 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 methyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 212°-214° 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-2343817238154b91a71b7b1a643bedcf
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346030

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