Phosphorus oxychloride → 4-Chloro-2,8-dimethyl-8-phenyl-5,6,7,8-tetrahydroquinazoline
Reaktionsgleichung
[CH3:1][C:2]1[N:11]=[C:10](O)[C:9]2[CH2:8][CH2:7][CH2:6][C:5]([CH3:19])([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:4]=2[N:3]=1.P(Cl)(Cl)([Cl:22])=O>>[Cl:22][C:10]1[C:9]2[CH2:8][CH2:7][CH2:6][C:5]([CH3:19])([C:13]3[CH:18]=[CH:17][CH:16]=[CH:15][CH:14]=3)[C:4]=2[N:3]=[C:2]([CH3:1])[N:11]=1Komponenten
3
Versuchsvorschrift
A mixture of 2,8-dimethyl-8-phenyl-5,6,7,8-tetrahydro-quinazolin-4-ol (4 g, 16 mmol) and 25 mL of phosphorous oxychloride was heated under reflux for 2 hours, concentrated under reduced pressure and ice, water and dichloromethane were added. The mixture was basified with aqueous sodium carbonate and the organic layer was dried (sodium sulfate) and evaporated to afford 4.4 g of 4-chloro-2,8-dimethyl-8-phenyl-5,6,7,8-tetrahydroquinazoline as an oil.
Aufarbeitung
- temperaturewas heated
- temperatureunder reflux for 2 hours
- concentrationconcentrated under reduced pressure and ice, water and dichloromethane
- additionwere added
- dry with materialthe organic layer was dried (sodium sulfate)
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-b398dc5a99ab4f8e82ea04d69a9a9470
- Quelldatensatz
- uspto-grants-2007_05
- Patentnummer
- US07223767B2
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