Dimethyl Sulfate → 1-methyl-4-nitro-1H-pyrazole
Reaktionsgleichung
[N+:1]([C:4]1[CH:5]=[N:6][NH:7][CH:8]=1)([O-:3])=[O:2].S(OC)(O[CH3:13])(=O)=O>[OH-].[Na+]>[CH3:13][N:6]1[CH:5]=[C:4]([N+:1]([O-:3])=[O:2])[CH:8]=[N:7]1Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
To a 500 mL round bottom flask containing 4-nitro-1-H-pyrazole (5 g, 44.2 mmol) was added sodium hydroxide (1M, 200 mL) and dimethyl sulfate (31 mL, 330 mmol). The mixture was stirred at room temperature for 72 h and the mixture was extracted with CH2Cl2 (2×150 mL). The organic layer was separated and the solvent was distilled off to yield 1-methyl-4-nitro-1H-pyrazole as a white solid (4.30 g, 76%).
Aufarbeitung
- extractionthe mixture was extracted with CH2Cl2 (2×150 mL)
- customThe organic layer was separated
- distillationthe solvent was distilled off
Quellen und Nachweise
- ORD-Eintrag
- ord-5d0693790be74daa9232a9d7cfdd9134
- Quelldatensatz
- uspto-grants-2016_05
- Patentnummer
- US09328106B2
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