Methyl iodide → HCID 67711340, Verbindung

HRID 974860Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 974860
[H-].[Na+].[CH2:3]([O:5][C:6]([CH:8]1[NH:13][C:12](=[O:14])[CH:11]([CH2:15][CH:16]([CH3:18])[CH3:17])[N:10]([O:19][CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][O:21]2)[C:9]1=[O:26])=[O:7])[CH3:4].[CH3:27]I.[Cl-].[NH4+]>CN(C)C=O>[CH2:3]([O:5][C:6]([C:8]1([CH3:27])[NH:13][C:12](=[O:14])[CH:11]([CH2:15][CH:16]([CH3:18])[CH3:17])[N:10]([O:19][CH:20]2[CH2:25][CH2:24][CH2:23][CH2:22][O:21]2)[C:9]1=[O:26])=[O:7])[CH3:4]

Komponenten

6

Edukt 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 25517Ammonium ChlorideHCID 19969552HCID 19969552, Verbindung

Produkt 1

HCID 67711340HCID 67711340, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

1.04 g of 60% sodium hydride was added to 100 ml of 9.67 g of 3-ethoxycarbonyl-6-isobutyl-1-(2-tetrahydropyranyloxy)piperazine-2,5-dione in anhydrous N,N-dimethylformamide, on ice cooling, and the mixture was stirred for 10 minutes. Thereto was added 3.5 ml of methyl iodide. The mixture was stirred at room temperature for 5 hours. The reaction mixture was ice-cooled and poured into an aqueous solution saturated with ammonium chloride. The mixture was extracted with ethyl acetate. The extract was washed three times with an aqueous solution saturated with sodium chloride, dried with anhydrous magnesium sulfate, and subjected to distillation to remove the solvent to obtain 8.53 g of (3RS,6SR)-3-ethoxycarbonyl-6-isobutyl-3-methyl-1-(2-tetrahydropyranyloxy)piperazine-2,5-dione as a brown oily substance.

Aufarbeitung

  1. stirringThe mixture was stirred at room temperature for 5 hours
  2. temperaturecooled
  3. extractionThe mixture was extracted with ethyl acetate
  4. washThe extract was washed three times with an aqueous solution saturated with sodium chloride
  5. dry with materialdried with anhydrous magnesium sulfate
  6. distillationsubjected to distillation
  7. customto remove the solvent

Quellen und Nachweise

ORD-Eintrag
ord-129dbc3c4365457083ae4e7b63dc04b8
Quelldatensatz
uspto-grants-1997_03
Patentnummer
US05607934

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