Reaktionsgleichung
[N:1]1[CH:6]=[CH:5][C:4]([C:7]([OH:9])=[O:8])=[CH:3][N:2]=1.OS(O)(=O)=O.[CH2:15](O)[CH3:16]>>[CH2:15]([O:8][C:7]([C:4]1[CH:5]=[CH:6][N:1]=[N:2][CH:3]=1)=[O:9])[CH3:16]Komponenten
4
Versuchsvorschrift
To pyridazine-4-carboxylic acid (1.0 g, 8.1 mmol) in ethanol (10 mL) was added concentrated H2SO4 (4.2 mL) and then heated at reflux for 5 hours. The reaction mixture was cooled, concentrated in vacuo and basified with saturated Na2CO3. After filtration, the aqueous was extracted with ethyl acetate, dried over anhydrous Na2SO4, filtered and concentrated to give the title product as a dark yellow oil (970 mg, 79%).
Aufarbeitung
- temperatureheated
- temperatureat reflux for 5 hours
- temperatureThe reaction mixture was cooled
- concentrationconcentrated in vacuo
- filtrationAfter filtration
- extractionthe aqueous was extracted with ethyl acetate
- dry with materialdried over anhydrous Na2SO4
- filtrationfiltered
- concentrationconcentrated
Quellen und Nachweise
- ORD-Eintrag
- ord-b84e4f7eedb348819d43d40a83292036
- Quelldatensatz
- uspto-grants-2010_03
- Patentnummer
- US07678796B2
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