Reaktionsgleichung
S(Cl)([Cl:3])=O.[CH3:5][O:6][C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15]O)[N:10]=1)=[O:8]>>[CH3:5][O:6][C:7]([C:9]1[CH:14]=[CH:13][CH:12]=[C:11]([CH2:15][Cl:3])[N:10]=1)=[O:8]Komponenten
3
Versuchsvorschrift
5 ml of thionyl chloride is slowly added to 2.50 g of 6-(hydroxymethyl)-2-pyridinecarboxylic acid methyl ester at 0° C. under nitrogen and stirred for 1 hour. The reaction mixture is concentrated by evaporation in a vacuum. The thus obtained residue is mixed with 15 ml of saturated sodium bicarbonate solution and extracted three times with 25 ml of toluene each. After the drying on sodium sulfate and filtration, it is concentrated by evaporation in a vacuum. 2.37 g of the title compound is obtained, which is further used without further purification.
Aufarbeitung
- concentrationThe reaction mixture is concentrated by evaporation in a vacuum
- additionThe thus obtained residue is mixed with 15 ml of saturated sodium bicarbonate solution
- extractionextracted three times with 25 ml of toluene each
- filtrationAfter the drying on sodium sulfate and filtration, it
- concentrationis concentrated by evaporation in a vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-3cf515ebee1844e3ba44c969d281b5a7
- Quelldatensatz
- uspto-grants-1996_09
- Patentnummer
- US05559134
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