Reaktion #1994846

Reaktionsgleichung

5-(4-chlorophenyl)-4-(3,5-dichloro-2-pyridyl)-6-methyl-2H-pyridazin-3-one

phosphorus oxychloride

→

3-chloro-5-(4-chlorophenyl)-4-(3,5-dichloro-2-pyridyl)-6-methylpyridazine

Ausbeute 67.8%

Reaktionsbedingungen

Aufarbeitung

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

Vorschrift

0.66 g of 5-(4-chlorophenyl)-4-(3,5-dichloro-2-pyridyl)-6-methyl-2H-pyridazin-3-one and 6 g of phosphorus oxychloride were mixed. The mixture was stirred for 2 hours on an oil bath of 110° C. The reaction mixture was allowed to cool to room temperature, then, concentrated under reduced pressure. To the resultant residue were added ethyl acetate and ice-cooled sodium bicarbonate water. 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. 0.67 g of the resultant residue was subjected to silica gel column chromatography, to obtain 0.47 g of 3-chloro-5-(4-chlorophenyl)-4-(3,5-dichloro-2-pyridyl)-6-methylpyridazine (hereinafter, described as compound (11) of the present invention.).

Quelle