Methanol → HCID 22768399, Verbindung

HRID 867064Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 867064
C(O[C:4]1[CH2:10][N:9]=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7]2[CH:17]=[C:18]([N+:21]([O-:23])=[O:22])[CH:19]=[CH:20][C:6]=2[N:5]=1)C.CO.O.[NH2:27][NH2:28]>O>[NH:27]([C:4]1[CH2:10][N:9]=[C:8]([C:11]2[CH:16]=[CH:15][CH:14]=[CH:13][CH:12]=2)[C:7]2[CH:17]=[C:18]([N+:21]([O-:23])=[O:22])[CH:19]=[CH:20][C:6]=2[N:5]=1)[NH2:28]

Komponenten

5

Edukt 3

HCID 887MethanolHCID 24654Hydrazine hydrate (1:1)HCID 203172642-ethoxy-7-nitro-5-phenyl-3H-1,4-benzodiazepine

Produkt 1

HCID 22768399HCID 22768399, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

To a solution of 0.25 part of 2-ethoxy-7-nitro-5-phenyl-3H-1,4-benzodiazepine in 8 parts by volume of methanol is added 0.2 part by volume of hydrazine hydrate (100%) with stirring and the stirring is continued at room temperature for further 2.5 hours. To the reaction mixture is added water, followed by extraction with chloroform. Chloroform layer is washed with water and dried over anhydrous sodium sulfate, followed by distillation of the solvent. Treatment of the residue with n-hexane gives 2-hydrazino-7-nitro-5-phenyl-3H-1,4-benzodiazepine as orange crystalline powder. The product is treated with acetone, whereupon 2-(2-isopropylidenehydrazino)-7-nitro-5-phenyl-3H-1,4-benzodiazepine is obtained as pale yellow crystals melting at 203°-205° C.

Aufarbeitung

  1. extractionfollowed by extraction with chloroform
  2. washChloroform layer is washed with water
  3. dry with materialdried over anhydrous sodium sulfate
  4. distillationfollowed by distillation of the solvent

Quellen und Nachweise

ORD-Eintrag
ord-2a5a15a3c4e14cdab7e48d0bad45025c
Quelldatensatz
uspto-grants-1978_07
Patentnummer
US04102881

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