Potassium Cyanide → HCID 54376820, Verbindung

HRID 1154461Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1154461
[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18][CH2:19][CH3:20])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[C-]#N.[K+].[O:28]1[CH2:33]CC(O)[CH2:30][CH2:29]1>>[Cl:1][C:2]1[C:7]2[C:8](=[O:24])[N:9]3[CH2:23][CH2:22][CH2:21][C@H:10]3[C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18][CH:19]3[CH2:30][CH2:29][O:28][CH2:33][CH2:20]3)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1

Komponenten

4

Edukt 3

HCID 9032Potassium CyanideHCID 74956Tetrahydro-4H-pyran-4-ol2×HCID 53890667ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]-benzodiazepine-1-carboxylate

Produkt 1

HCID 54376820HCID 54376820, Verbindung

Versuchsvorschrift

A mixture of 3.45 g (10 mmol) of ethyl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate, 100 mg of powdered potassium cyanide and 10 g (100 mmol) of tetrahydro-2H-pyran-4-ol is heated at 140° for 20 hours, whereupon the excess tetrahydro-2H-pyran-4-ol is distilled off and the residue is taken up in chloroform. The solution is washed with water, dried over magnesium sulphate and evaporated. By crystallization from ethyl acetate there is obtained tetrahydro-2H pyran-4-yl (S)-8-chloro-11,12,13,13a-tetrahydro-9-oxo-9H-imidazo[1,5-a]pyrrolo[2,1-c][1,4]benzodiazepine-1-carboxylate of melting point 226°-227°.

Aufarbeitung

  1. distillationis distilled off
  2. washThe solution is washed with water
  3. dry with materialdried over magnesium sulphate
  4. customevaporated
  5. customBy crystallization from ethyl acetate

Quellen und Nachweise

ORD-Eintrag
ord-8e938dbe53b8473391568d2b6a5733e5
Quelldatensatz
uspto-grants-1984_12
Patentnummer
US04489003

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