Phosphorus oxychloride → 4-Chloro-2,8-dimethyl-8-phenyl-5,6,7,8-tetrahydroquinazoline

HRID 1354096Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1354096
[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]=1

Komponenten

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

  1. temperaturewas heated
  2. temperatureunder reflux for 2 hours
  3. concentrationconcentrated under reduced pressure and ice, water and dichloromethane
  4. additionwere added
  5. dry with materialthe organic layer was dried (sodium sulfate)
  6. customevaporated

Quellen und Nachweise

ORD-Eintrag
ord-b398dc5a99ab4f8e82ea04d69a9a9470
Quelldatensatz
uspto-grants-2007_05
Patentnummer
US07223767B2

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