Phosphorus oxychloride → 4-Chloro-6-fluoropyrido[3,2-D]pyrimidine
Reaktionsgleichung
[F:1][C:2]1[CH:3]=[CH:4][C:5]2[N:6]=[CH:7][NH:8][C:9](=O)[C:10]=2[N:11]=1.O=P(Cl)(Cl)[Cl:15]>>[Cl:15][C:9]1[C:10]2[N:11]=[C:2]([F:1])[CH:3]=[CH:4][C:5]=2[N:6]=[CH:7][N:8]=1Komponenten
3
Versuchsvorschrift
A suspension of 6-fluoro-3H-pyrido[3,2-d]pyrimid-4-one (0.20 g, 1.21 mmol) in POCl3 (30mL) is heated under reflux with stirring until homogeneous (2 h), and then for a further 1 h. Excess POCl3 is removed under reduced pressure, and the residue is partitioned between CH2Cl2 and saturated aqueous NaHCO3. Workup of the organic portion gives crude 4-chloro-6-fluoropyrido[3,2-d]pyrimidine (100%) as an unstable white solid which is used directly in the next step.
Aufarbeitung
- temperatureis heated
- temperatureunder reflux
- waitfor a further 1 h
- customExcess POCl3 is removed under reduced pressure
- customthe residue is partitioned between CH2Cl2 and saturated aqueous NaHCO3
Quellen und Nachweise
- ORD-Eintrag
- ord-0f300b9610c847409472238646c218df
- Quelldatensatz
- uspto-grants-2004_03
- Patentnummer
- US06713484B2
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