Reaktion #1994843

Reaktionsgleichung

5-(4-chlorophenyl)-6-methyl-4-(2-pyrimidinyl)-2H-pyridazin-3-one

phosphorus oxychloride

→

3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2-pyrimidinyl)pyridazine

Ausbeute 72.1%

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturunder reflux
2. 2
   Temperaturwith heating
3. 3
   Einengenconcentrated under reduced pressure
4. 4
   workup.ADDITIONTo the resultant residue was added ethyl acetate and ice-
5. 5
   Temperaturcooled sodium bicarbonate water
6. 6
   workup.ADDITIONwas added
7. 7
   workup.STIRRINGThe mixture was stirred for about 5 minutes at room temperature
8. 8
   Sonstigeliquid-separated
9. 9
   WaschenThe organic layer was washed with brine
10. 10
    Trocknendried over anhydrous magnesium sulfate
11. 11
    Einengenconcentrated under reduced pressure

Vorschrift

0.64 g of 5-(4-chlorophenyl)-6-methyl-4-(2-pyrimidinyl)-2H-pyridazin-3-one and 10.4 g of phosphorus oxychloride were mixed. The mixture was stirred for 2 hours under reflux with heating. The reaction mixture was allowed to cool to room temperature, then, concentrated under reduced pressure. To the resultant residue was added ethyl acetate and ice-cooled sodium bicarbonate water was added. The mixture was stirred for about 5 minutes at room temperature, then, liquid-separated. The organic layer was washed with brine, and dried over anhydrous magnesium sulfate, then, concentrated under reduced pressure. 0.56 g of the resultant residue was subjected to silica gel column chromatography, to obtain 0.49 g of 3-chloro-5-(4-chlorophenyl)-6-methyl-4-(2-pyrimidinyl)pyridazine (hereinafter, described as compound (6) of the present invention (6).).

Quelle