Phosphorus oxychloride → 4-Chloropyrido[2,3-d]pyrimidine
Reaktionsgleichung
[N:1]1[C:6]2[N:7]=[CH:8][CH:9]=[CH:10][C:5]=2[C:4](=O)[NH:3][CH:2]=1.O=P(Cl)(Cl)[Cl:14]>>[Cl:14][C:4]1[C:5]2[CH:10]=[CH:9][CH:8]=[N:7][C:6]=2[N:1]=[CH:2][N:3]=1Komponenten
3
Versuchsvorschrift
A mixture of 17.8 g of Pyrido[2,3-d]pyrimidin4(3H)one and 200 mL of POCl3 was stirred under reflux for one hour. Excess POCl3 was removed under vacuum, and then CH2Cl2, ice, and water were added. A black solid dissolved slowly. The organic layer was then separated, washed with aqueous NaHCO3, and dried over Na2SO4. Solvent was then removed under vacuum to leave a yellow solid, which was recrystallized from toluene/hexane. M.P. 137° dec.
Aufarbeitung
- temperatureunder reflux for one hour
- customExcess POCl3 was removed under vacuum
- additionCH2Cl2, ice, and water were added
- dissolutionA black solid dissolved slowly
- customThe organic layer was then separated
- washwashed with aqueous NaHCO3
- dry with materialdried over Na2SO4
- customSolvent was then removed under vacuum
- customto leave a yellow solid, which
- customwas recrystallized from toluene/hexane
Quellen und Nachweise
- ORD-Eintrag
- ord-92255a965cad4addb14d89dee2ad5945
- Quelldatensatz
- uspto-grants-1991_07
- Patentnummer
- US05034393
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