Pyridazine-4-carboxylic Acid → 3-Methylpyridazine-4-carboxylic acid

HRID 550528

Reaktionsgleichung

Reaktionsgleichung von HRID 550528
[N:1]1[CH:6]=[CH:5][C:4]([C:7]([OH:9])=[O:8])=[CH:3][N:2]=1.CO.[CH2:12](Cl)Cl>>[CH3:12][C:3]1[N:2]=[N:1][CH:6]=[CH:5][C:4]=1[C:7]([OH:9])=[O:8]

Komponenten

3

Edukt 2

HCID 2761046Pyridazine-4-carboxylic AcidHCID 21226129Dichloromethane methanol

Produkt 1

HCID 534147303-Methylpyridazine-4-carboxylic acid

Versuchsvorschrift

To a solution of 4-pyridazinecarboxylic acid (490 mg, 3.9 mmol) in MeOH/DCM (20/10 ml) was added at 0° C. trimethylsilildiazomethane (25.5 mmol). The solution was warm at r.t. and stirred overnight. Volatiles were evaporated in vacuo, the crude dissolved in DCM, washed with NaHCO3 satured and dried over Na2SO4. After filtration and concentration to dryness in vacuo, the crude was purified by column chromatography (DCM:MeOH=98 to 2) to give 400 mg of the title compound.

Aufarbeitung

  1. customVolatiles were evaporated in vacuo
  2. dissolutionthe crude dissolved in DCM
  3. washwashed with NaHCO3
  4. dry with materialdried over Na2SO4
  5. filtrationAfter filtration and concentration to dryness in vacuo
  6. customthe crude was purified by column chromatography (DCM:MeOH=98 to 2)

Quellen und Nachweise

ORD-Eintrag
ord-3350765f503146e58941656a0524ca59
Quelldatensatz
uspto-grants-2011_05
Patentnummer
US07947683B2

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