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Methyl iodide → ethyl 5-methoxy-1H-pyrazole-3-carboxylate

HRID 1181574
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1181574
[CH2:1]([O:3][C:4]([C:6]1[CH:10]=[C:9]([OH:11])[NH:8][N:7]=1)=[O:5])[CH3:2].[C:12](=O)([O-])[O-].[Cs+].[Cs+].IC>CN(C)C=O>[CH2:1]([O:3][C:4]([C:6]1[CH:10]=[C:9]([O:11][CH3:12])[NH:8][N:7]=1)=[O:5])[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 6328Methyl iodideHCID 10796Cesium carbonateHCID 178469373HCID 178469373, Verbindung

Produkt 1

HCID 178469331ethyl 5-methoxy-1H-pyrazole-3-carboxylateAusbeute 38 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Versuchsvorschrift

5-Hydroxy-1H-pyrazole-3-carboxylic acid ethyl ester (300 mg, 1.92 mmol) was dissolved in anhydrous N,N-dimethylformamide (DMF) (35 ml) and cesium carbonate (626 mg, 1.92 mmol) was added. The resulting suspension was treated with iodomethane (120 μl, 273 mg, 1.92 mmol) and stirred for 12 h at room temperature. The reaction mixture was quenched with saturated potassium hydrogen sulfate solution and extracted with ethyl acetate (3×100 ml). The combined organic layers were washed with water (50 ml) and brine (50 ml). The extract was dried over sodium sulfate, evaporated and the crude product was purified by column chromatography on silica gel. Elution with ethyl acetate/n-heptane (1:3) yielded 124 mg (38%) of a white solid.

Aufarbeitung

  1. customThe reaction mixture was quenched with saturated potassium hydrogen sulfate solution
  2. extractionextracted with ethyl acetate (3×100 ml)
  3. washThe combined organic layers were washed with water (50 ml) and brine (50 ml)
  4. dry with materialThe extract was dried over sodium sulfate
  5. customevaporated
  6. customthe crude product was purified by column chromatography on silica gel
  7. washElution with ethyl acetate/n-heptane (1:3)

Quellen und Nachweise

ORD-Eintrag
ord-c81f16c948c749b3a200bd8f09761682
Quelldatensatz
uspto-grants-2007_10
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07285569B2

Notizen zur Reaktion

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