Reaktionsgleichung
[C:1]([OH:10])(=[O:9])[C:2]1[CH:7]=[CH:6][CH:5]=[N+:4]([O-])[CH:3]=1.C(N(CC)CC)C.O=P(Cl)(Cl)[Cl:20]>>[Cl:20][C:3]1[N:4]=[CH:5][CH:6]=[CH:7][C:2]=1[C:1]([OH:10])=[O:9]Komponenten
Reaktionsbedingungen
- Temperatur
- 100 °C
Versuchsvorschrift
70 gm. of nicotinic acid-N-oxide was suspended in 300 ml of POCl3. Then 50 gm. of triethyl amine was added drop by drop at room temperature, whereby the nicotinic acid-N-oxide dissolved at about 50° C. (the temperature rise occured due to an exothermic reaction). Then the solution was heated in a water bath at 100° C. for another 4 hours. The main quantity of excess phosphorus oxychloride was distilled off under vacuum. The residue was allowed to flow into water at a temperature below 40° C. After addition of diluted caustic soda solution, the 2-chloronicotnic acid precipitated at a pH value of 2.0 to 2.5. The product had a melting point of 173° to 175° C. (Kofler). The product (2-chloronicotinic acid) yield amounted to 65 to 70 percent of theory.
Aufarbeitung
- customoccured due to an exothermic reaction)
- distillationThe main quantity of excess phosphorus oxychloride was distilled off under vacuum
- customto flow into water at a temperature below 40° C
- additionAfter addition of diluted caustic soda solution
- customthe 2-chloronicotnic acid precipitated at a pH value of 2.0 to 2.5
Quellen und Nachweise
- ORD-Eintrag
- ord-25577deb5cfc42458dc17143a4e4697c
- Quelldatensatz
- uspto-grants-1979_03
- Patentnummer
- US04144238
Verknüpfte Notizen
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