Methyl iodide → HCID 5302363, Verbindung

HRID 559042Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 559042
[H-].[Na+].[N+:3]([C:6]1[CH:10]=[CH:9][NH:8][CH:7]=1)([O-:5])=[O:4].I[CH3:12].[H][H]>CCCCCC.CN(C=O)C.CCOC(C)=O.O>[CH3:12][N:8]1[CH:9]=[CH:10][C:6]([N+:3]([O-:5])=[O:4])=[CH:7]1

Komponenten

9

Edukt 4

HCID 6328Methyl iodideHCID 24758Sodium hydrideHCID 1458133-NitropyrroleHCID 178418361HCID 178418361, Verbindung

Produkt 1

HCID 5302363HCID 5302363, VerbindungAusbeute 87,8 %

Reagenzien, Katalysatoren, Lösungsmittel 4

HCID 962WaterLösungsmittelHCID 6228DimethylformamideLösungsmittelHCID 8058HexaneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To sodium hydride (300 mg, 60% in mineral oil, 7.50 mmol) in a flask, which was washed with hexane twice, a solution of 3-nitropyrrole (500 mg, 4.46 mmol) and iodomethane (0.560 mL, 8.97 mmol) in DMF (4 mL) was added. Hydrogen gas evolved. The mixture was then stirred at room temperature for 20 h. Water and EtOAc were added. Organic phase was separated, washed with water, dried over Na2SO4, concentrated in vacuo to give 1-methyl-3-nitro-1H-pyrrole (494 mg).

Aufarbeitung

  1. customOrganic phase was separated
  2. washwashed with water
  3. dry with materialdried over Na2SO4
  4. concentrationconcentrated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-9cf79b0d4fcd477cb1ddff31f12438c3
Quelldatensatz
uspto-grants-2011_11
Patentnummer
US08063058B2

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