Hydrazine hydrate (1:1) → 3-Amino-5-phenyl-1,3-dihydro-1,4-benzodiazepin-2-one

HRID 258089

Reaktionsgleichung

Reaktionsgleichung von HRID 258089
[C:1]1([C:7]2[C:13]3[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=3[NH:11][C:10](=[O:18])[CH:9]([N:19]3C(=O)C4=CC=CC=C4C3=O)[N:8]=2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.O.NN>O1CCCC1>[NH2:19][CH:9]1[N:8]=[C:7]([C:1]2[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=2)[C:13]2[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=2[NH:11][C:10]1=[O:18]

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 14800302(3RS)-1,3-dihydro-5-phenyl-3-phthalimido-2H-1,4-benzodiazepine-2-one

Produkt 1

HCID 42596493-Amino-5-phenyl-1,3-dihydro-1,4-benzodiazepin-2-oneAusbeute 67,4 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

A mixture of (3RS)-1,3-dihydro-5-phenyl-3-phthalimido-2H-1,4-benzodiazepine-2-one (8.2 g), hydrazine hydrate (1.08 g) and tetrahydrofuran (160 ml) was stirred for 1.0 hour at room temperature and heated under reflux for 1.5 hours. After the precipitates were filtered off, the filtrate was evaporated to small volume and the equivalent volume of diisopropyl ether was added thereto. The precipitates were collected by filtration to give (3RS)-1,3-dihydro-3-amino-5-phenyl-2H-1,4-benzodiazepine-2-one (3.64 g).

Aufarbeitung

  1. temperatureheated
  2. temperatureunder reflux for 1.5 hours
  3. filtrationAfter the precipitates were filtered off
  4. customthe filtrate was evaporated to small volume
  5. additionthe equivalent volume of diisopropyl ether was added
  6. filtrationThe precipitates were collected by filtration

Quellen und Nachweise

ORD-Eintrag
ord-bd8e9bfe2d904515a7486e9d40512fef
Quelldatensatz
uspto-grants-1993_11
Patentnummer
US05264433

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