Hydrochloric Acid → 5-Methyl-4-pyridazinecarboxylic acid
Reaktionsgleichung
[CH3:1][C:2]1[C:3]([C:8]([O:10]CC)=[O:9])=[CH:4][N:5]=[N:6][CH:7]=1.[OH-].[Na+].Cl>O.C1COCC1>[CH3:1][C:2]1[C:3]([C:8]([OH:10])=[O:9])=[CH:4][N:5]=[N:6][CH:7]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Reaktionsbedingungen
- Temperatur
- 60 °C
Versuchsvorschrift
To a solution of ethyl 5-methylpyridazine-4-carboxylate (240 mg, 1.4 mmol) in H2O/THF was added 7.5 N aq. NaOH (1.25 eq, 0.25 mL) and the mixture was stirred for 1 hour at 60° C. Concentrated HCl was added to pH 2 and subsequently the volatiles were removed in vacuo. The residue was first stirred with EtOAc and the solids were collected by filtration. Then stirred with THF and the solids were again collected by filtration. The solids were extracted with MeOH and removal of the volatiles afforded 5-methylpyridazine-4-carboxylic acid (358 mg) as a brown solid.
Aufarbeitung
- customsubsequently the volatiles were removed in vacuo
- stirringThe residue was first stirred with EtOAc
- filtrationthe solids were collected by filtration
- stirringThen stirred with THF
- filtrationthe solids were again collected by filtration
- extractionThe solids were extracted with MeOH and removal of the volatiles
Quellen und Nachweise
- ORD-Eintrag
- ord-703e97f0e652443db16f0acbebce704f
- Quelldatensatz
- uspto-grants-2012_04
- Patentnummer
- US08148380B2
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