Reacción #56172

Ecuación de reacción

3-chloro-6-(3-methyl-5-hydroxy-1-pyrazolyl)-pyridazine

phosphorus oxychloride

dimethyl aniline

→

3-chloro-6-(3-methyl-5-chloro-1-pyrazolyl)-pyridazine

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.ADDITIONare dropped
2. 2
   workup.STIRRINGthe reaction mixture is stirred at room temperature for one hour
3. 3
   Otrofor 2 hours
4. 4
   OtroExcess of the phosphorus oxychloride is evaporated under reduced pressure
5. 5
   workup.ADDITIONthe residue is poured into water
6. 6
   FiltraciónThe separated precipitate is filtered
7. 7
   Lavadowashed with water
8. 8
   Otrodried

Procedimiento

To the mixture of 12.6 /0.04 moles/ of 3-chloro-6-(3-methyl-5-hydroxy-1-pyrazolyl)-pyridazine and 48 ml of phosphorus oxychloride, 7.28 g /0.04 moles/ of dimethyl aniline are dropped under stirring at 0° C. during half an hour, then the reaction mixture is stirred at room temperature for one hour and at boiling temperature for 2 hours. Excess of the phosphorus oxychloride is evaporated under reduced pressure, then the residue is poured into water and set aside overnight. The separated precipitate is filtered, washed with water and dried. Yield: 10.5 g (93%); m.p.: 123°-126° C.

Fuente