Reaktion #602750

Reaktionsgleichung

6-chloro-2-phenyl-3-(pyridazin-4-yl)imidazo[1,2-b]pyridazine

1-isopropylpiperazine

hydrochloric acid

→

solid

Ausbeute 83.4%

2-phenyl-6-(4-isopropylpiperazin-1-yl)-3-(pyridazin-4-yl)imidazo[1,2-b]pyridazine

Ausbeute 83.4%

Lösungsmittel

pentanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   TemperaturThe mixture is cooled
2. 2
   WaschenThis solution is washed with diethyl ether
3. 3
   ExtraktionThe product is finally extracted with dichloromethane
4. 4
   Trocknenthe organic phase is dried over sodium sulfate
5. 5
   Filtrationfiltered
6. 6
   Einengenconcentrated under reduced pressure
7. 7
   SonstigeA brown oil is obtained
8. 8
   Sonstigewhich is chromatographed on silica gel, elution
9. 9
   workup.ADDITIONbeing carried out with a mixture of aqueous ammonia, methanol and dichloromethane (0.4/4/96)

Vorschrift

The mixture of 0.45 g (1.5 mmol) of 6-chloro-2-phenyl-3-(pyridazin-4-yl)imidazo[1,2-b]pyridazine and 0.38 g (2.9 mmol) of 1-isopropylpiperazine in 6 ml of pentanol is heated in a sealed tube at 150° C. for 2 days. The mixture is cooled and poured into a 1N aqueous solution of hydrochloric acid. This solution is washed with diethyl ether and then basified using an aqueous solution of sodium hydroxide. The product is finally extracted with dichloromethane, and the organic phase is dried over sodium sulfate, filtered and concentrated under reduced pressure. A brown oil is obtained, which is chromatographed on silica gel, elution being carried out with a mixture of aqueous ammonia, methanol and dichloromethane (0.4/4/96), to give 0.50 g of a solid.

Quelle