Water → 1-methyl-4-nitro-1H-pyrazole

HRID 84801

Reaktionsgleichung

Reaktionsgleichung von HRID 84801
[N+:1]([C:4]1[CH:5]=[N:6][NH:7][CH:8]=1)([O-:3])=[O:2].I[CH3:10].[H-].[Na+].O>CN(C=O)C.CCOC(C)=O>[CH3:10][N:6]1[CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:8]=[N:7]1

Komponenten

7

Edukt 4

HCID 962WaterHCID 6328Methyl iodideHCID 163764-nitro-1H-pyrazoleHCID 24758Sodium hydride

Produkt 1

HCID 198951-methyl-4-nitro-1H-pyrazoleAusbeute 87,3 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 6228DimethylformamideLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Versuchsvorschrift

To a solution of 4-nitro-1H-pyrazole (1.13 g, 10.0 mmol) and iodomethane (1.25 mL, 20.0 mmol) in DMF (12 mL), NaH (60% in mineral oil, 0.600 g, 15.0 mmol) was added. The mixture was stirred for 18 h. Water and EtOAc were added. The organic phase was separated, washed with water, dried over Na2SO4, concentrated in vacuo to give 1-methyl-4-nitro-1H-pyrazole as a solid (1.11 g).

Aufarbeitung

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

Quellen und Nachweise

ORD-Eintrag
ord-70caa30616674d57aacfc9d4bd670837
Quelldatensatz
uspto-grants-2014_09
Patentnummer
US08846928B2

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