Ethylene Glycol → HCID 20518108, Verbindung

HRID 67322

Reaktionsgleichung

Reaktionsgleichung von HRID 67322
[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-]#N.[K+].C(O)C[OH:27]>C(Cl)(Cl)Cl>[OH:27][CH2:21][CH2:20][O:19][C:17]([C:16]1[N:15]=[CH:14][N:5]2[C:6]3[CH:13]=[CH:12][CH:11]=[CH:10][C:7]=3[C:8](=[O:9])[N:2]([CH3:1])[CH2:3][C:4]=12)=[O:18]

Komponenten

5

Edukt 3

HCID 174Ethylene GlycolHCID 9032Potassium CyanideHCID 127597Ro 14-7437

Produkt 1

HCID 20518108HCID 20518108, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6212ChloroformLösungsmittel

Reaktionsbedingungen

Temperatur
130 °C

Versuchsvorschrift

A mixture of 1.42 g (5 mmol) of ethyl 5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate, 100 mg of potassium cyanide and 10 ml of ethyleneglycol is stirred at 130° C. for 6 hours, subsequently diluted with chloroform, washed with water, dried over magnesium sulphate and evaporated. After recrystallisation of the residue from ethyl acetate, there is obtained 2-hydroxyethyl-5,6-dihydro-5-methyl-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate of melting point 222°-223° C.

Aufarbeitung

  1. washwashed with water
  2. dry with materialdried over magnesium sulphate
  3. customevaporated
  4. customAfter recrystallisation of the residue from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-c189917d6745426ea292015eab11fd14
Quelldatensatz
uspto-grants-1982_08
Patentnummer
US04346030

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