Reaktion #40849

Reaktionsgleichung

1-methyl-5,6-diphenyl-1H-pyrimidin-2-one

1-Methyl-5,6-diphenyl-1H-pyrimidin-2-one

phosphorus oxychloride

phosphorus pentachloride

→

title compound

2-Chloro-4,5-diphenyl-pyrimidine

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeThe excess amount of phosphorus oxychloride was removed under reduced pressure and cold water
2. 2
   workup.ADDITIONwas added to the residue
3. 3
   ExtraktionThe resulting precipitate was extracted with CH2Cl2
4. 4
   WaschenThe organic layer was washed with brine
5. 5
   Trocknendried over MgSO4
6. 6
   Einengenconcentrated in vacuo
7. 7
   SonstigeThe residue was purified by column chromatography (20% ethyl acetate in hexane)

Vorschrift

A solution of 1-methyl-5,6-diphenyl-1H-pyrimidin-2-one (106, 314 mg, 1.20 mmol), phosphorus oxychloride (0.6 ml, 6.4 mmol) and phosphorus pentachloride (55 mg, 0.26 mmol) was heated at 120° C. for 3 hours. The excess amount of phosphorus oxychloride was removed under reduced pressure and cold water was added to the residue. The resulting precipitate was extracted with CH2Cl2. The organic layer was washed with brine, and dried over MgSO4, and concentrated in vacuo. The residue was purified by column chromatography (20% ethyl acetate in hexane) to produce the title compound as a white solid.

Quelle