Phosphorus oxychloride → 5-Chloro-1,6-naphthyridine
Reaktionsgleichung
[N:1]1[C:10]2[CH:9]=[CH:8][N:7]=[C:6](O)[C:5]=2[CH:4]=[CH:3][CH:2]=1.P(Cl)(Cl)([Cl:14])=O>>[Cl:14][C:6]1[N:7]=[CH:8][CH:9]=[C:10]2[C:5]=1[CH:4]=[CH:3][CH:2]=[N:1]2Komponenten
3
Reaktionsbedingungen
- Temperatur
- 80 °C
Versuchsvorschrift
The product from Example 36d (0.250 g, 1.71 mmol) was combined with phosphorous oxychloride (4 mL) and heated under a nitrogen atmosphere at 80° C. for 18.5 h followed by vacuum distillation to remove the volatiles. The residue was slurried with ice and made basic (pH 7-8) with concentrated ammonium hydroxide. The title compound was collected by vacuum filtration, water washed and dried under vacuum to give a gray solid (0.245 g, 87%) sufficiently pure for use as isolated.
Aufarbeitung
- distillationfollowed by vacuum distillation
- customto remove the volatiles
- filtrationThe title compound was collected by vacuum filtration, water
- washwashed
- customdried under vacuum
Quellen und Nachweise
- ORD-Eintrag
- ord-37b0ea41be9c41638601733c59d369dd
- Quelldatensatz
- uspto-grants-2012_08
- Patentnummer
- US08236950B2
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