Reaktion #56174

Reaktionsgleichung

3-chloro-6-(3,5-dimethyl-1-pyrazolyl)-pyridazine

ethanol

methyl hydrazine

→

3-(1-methylhydrazino)-6-(3,5-dimethyl-1-pyrazolyl)-pyridazine

Lösungsmittel

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis heated
2. 2
   Temperaturto reflux for 9 hours
3. 3
   Temperaturafter cooling the mixture
4. 4
   ExtraktionThe solution is extracted with 3×50 ml of chloroform
5. 5
   Trocknenthe combined organic phases are dried over magnesium sulphate
6. 6
   SonstigeAfter evaporation the residue
7. 7
   Sonstigeis recrystallized from a 3:1 mixture of isopropanol and petroleum ether

Vorschrift

A mixture of 4.17 g (0.02 moles) of 3-chloro-6-(3,5-dimethyl-1-pyrazolyl)-pyridazine, 42 ml of ethanol and 2.3 g (0.05 moles) of methyl hydrazine is heated to reflux for 9 hours, and after cooling the mixture is poured into 100 ml of water. The solution is extracted with 3×50 ml of chloroform and the combined organic phases are dried over magnesium sulphate. After evaporation the residue is recrystallized from a 3:1 mixture of isopropanol and petroleum ether. Yield: 1.9 g (44.5%); m.p.: 93°-94° C.

Quelle