Methyl iodide → 1H-1,4-Benzodiazepine

HRID 441398

Reaktionsgleichung

Reaktionsgleichung von HRID 441398
Cl[C:2]1[CH:3]=[CH:4][C:5]2[N:11]3C(CON)=NN=[C:10]3[CH2:9][N:8]=[C:7](C3C=CC=CC=3)[C:6]=2[CH:24]=1.[H-].[Na+].CI>CN(C)C=O>[NH:11]1[C:5]2[CH:4]=[CH:3][CH:2]=[CH:24][C:6]=2[CH:7]=[N:8][CH:9]=[CH:10]1

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 126124268-chloro-1-[(aminooxy)methyl]6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine

Produkt 1

HCID 1484311H-1,4-Benzodiazepine

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

A stirred solution of 8-chloro-1-[(aminooxy)methyl]6-phenyl-4H-s-triazolo[4,3-a][1,4]benzodiazepine (0.02 mole) in dry dimethylformamide (50 ml.) is cooled in an ice bath under nitrogen and treated successively with a 57% mineral oil suspension of sodium hydride (0.84 g,. 0.02 mole) and methyliodide (0.02 mole). The mixture is allowed to come slowly to ambient temperature and stand for 18 hours. It is then concentrated in vacuo. The residue is chromatographed on silica gel with methanol to give 8-chloro-1-[[(methylamino)oxy]methyl]6-phenyl-4H-s-triazolo]4,3-a][1,4]benzodiazepine.

Aufarbeitung

  1. customto come slowly to ambient temperature
  2. concentrationIt is then concentrated in vacuo
  3. customThe residue is chromatographed on silica gel with methanol

Quellen und Nachweise

ORD-Eintrag
ord-d01ab87d9aa44073b1d7ec8d3cec7ccd
Quelldatensatz
uspto-grants-1977_08
Patentnummer
US04039551

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