Methyl iodide → HCID 20396007, Verbindung

HRID 261061Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 261061
[Cl:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][NH:11][C:10](=[O:14])[CH2:9]2)[CH:5]=[N:4][CH:3]=1.[H-].[Na+].[CH3:17]I>CN(C)C=O.C1(C)C=CC=CC=1.O>[Cl:1][C:2]1[N:7]=[C:6]([N:8]2[CH2:13][CH2:12][N:11]([CH3:17])[C:10](=[O:14])[CH2:9]2)[CH:5]=[N:4][CH:3]=1

Komponenten

7

Edukt 3

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 203960024-(6-Chloropyrazin-2-yl)piperazin-2-one

Produkt 1

HCID 20396007HCID 20396007, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 962WaterLösungsmittelHCID 1140TolueneLösungsmittelHCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

The product of Example 1 (2.13 g, 0.01 mole) and sodium hydride-oil suspension (50%, 0.50 g, 0.01 mole) are combined in 10 ml N,N-dimethylformamide and the stirred mixture treated with 0.65 ml (0.01 mole) of methyl iodide in 5 ml toluene. The mixture is stirred 1 hour at room temperature, diluted with water and extracted with toluene. The toluene extracts are washed with water, dried over sodium sulfate, filtered and concentrated in vacuo to give the crude product which is chromatographed on neutral (activity III) alumina. Elution with chloroform gives fractions containing 1.4 of a white solid which is recrystallized from n-butylchloride-cyclohexane to give white crystals of the title compound, mp 122°-123° C.

Aufarbeitung

  1. extractionextracted with toluene
  2. washThe toluene extracts are washed with water
  3. dry with materialdried over sodium sulfate
  4. filtrationfiltered
  5. concentrationconcentrated in vacuo
  6. customto give the crude product which
  7. customis chromatographed on neutral (activity III) alumina
  8. washElution with chloroform
  9. customgives fractions
  10. additioncontaining 1.4 of a white solid which
  11. customis recrystallized from n-butylchloride-cyclohexane

Quellen und Nachweise

ORD-Eintrag
ord-a15cf56d07ab40e8b21ff65fc97f3d36
Quelldatensatz
uspto-grants-1979_08
Patentnummer
US04163849

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