Sodium Methoxide → 7-Chloro-2-methoxy-5-phenyl-3H-1,4-benzodiazepine

HRID 649262

Reaktionsgleichung

Reaktionsgleichung von HRID 649262
[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([O:12]P(N3CCOCC3)(N3CCOCC3)=O)[CH2:9][N:8]=[C:7]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:33]=1.[CH3:34][O-].[Na+]>CO>[Cl:1][C:2]1[CH:3]=[CH:4][C:5]2[N:11]=[C:10]([O:12][CH3:34])[CH2:9][N:8]=[C:7]([C:27]3[CH:32]=[CH:31][CH:30]=[CH:29][CH:28]=3)[C:6]=2[CH:33]=1

Komponenten

4

Edukt 2

HCID 10942334Sodium MethoxideHCID 149078867-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepin

Produkt 1

HCID 6249427-Chloro-2-methoxy-5-phenyl-3H-1,4-benzodiazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 887MethanolLösungsmittel

Versuchsvorschrift

To a solution of 24.5 mg. (0.5 mmoles) of 7-chloro-2-di-(morpholino)phosphinyloxy-5-phenyl-3H-1,4-benzodiazepine in 5 ml. of methanol at room temperature was added 82 mg. (1.5 mmoles) of sodium methoxide. The mixture was left at room temperature overnight. Methanol was evaporated and the residue was slurried with ether. Insoluble salts were removed by filtration. The clear ether solution was evaporated. Crystallization of the residue from petroleum ether yielded a final product having a m.p. of 94°-97°.

Aufarbeitung

  1. customMethanol was evaporated
  2. customInsoluble salts were removed by filtration
  3. customThe clear ether solution was evaporated
  4. customCrystallization of the residue from petroleum ether

Quellen und Nachweise

ORD-Eintrag
ord-17f948a8d4fd4ffc89a4c301235b8fc8
Quelldatensatz
uspto-grants-1988_04
Patentnummer
US04739049

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