Delorazepam → EY5L4YP2FA

HRID 649266

Reaktionsgleichung

Reaktionsgleichung von HRID 649266
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[NH:11][C:10](=[O:12])[CH2:9][N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1.[H-].[Na+].[H-].[H][H].[O:26]1[CH2:31][CH2:30][N:29]([P:32](Cl)([N:34]2[CH2:39][CH2:38][O:37][CH2:36][CH2:35]2)=[O:33])[CH2:28][CH2:27]1>O1CCCC1>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([O:12][P:32]([N:34]3[CH2:35][CH2:36][O:37][CH2:38][CH2:39]3)([N:29]3[CH2:30][CH2:31][O:26][CH2:27][CH2:28]3)=[O:33])[CH2:9][N:8]=[C:7]([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][C:14]=3[Cl:19])[C:6]=2[CH:20]=1

Komponenten

7

Edukt 5

HCID 17925DelorazepamHCID 24758Sodium hydrideHCID 166653HydrideHCID 12506606Bis(morpholino)phosphinyl chlorideHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 12469774EY5L4YP2FA

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

To a stirred solution of 915 mg (3.0 mmoles) of 7-chloro-5-(2-chlorophenyl)-1,3-dihydro-2H-1,4-benzodiazepin-2-one in 10 ml of dry tetrahydrofuran was added 173 mg of a 50% dispersion as sodium hydride in oil (3.6 mmoles of hydride). The mixture was stirred at room temperature approximately 1 hr until hydrogen evolution stopped. Dimorpholinophosphinic chloride (1.5 g; 6.0 mmoles) was added and the resulting mixture was stirred at room temperature for 2 hrs. Insoluble salts were removed by filtration. Tetrahydrofuran was evaporated. The residue was crystallized from ethyl acetate to give colorless needles, mp 185°-187°.

Aufarbeitung

  1. customInsoluble salts were removed by filtration
  2. customTetrahydrofuran was evaporated
  3. customThe residue was crystallized from ethyl acetate
  4. customto give colorless needles, mp 185°-187°

Quellen und Nachweise

ORD-Eintrag
ord-bd6a255ccb4f44549fa79a6bec4b6f78
Quelldatensatz
uspto-grants-1988_04
Patentnummer
US04739049

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