반응 #602739

반응 방정식

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

5-benzyloctahydropyrrolo[3,4-c]pyrrole

hydrochloric acid

→

solid

수율 87.2%

6-(5-benzylhexahydropyrrolo[3,4-c]pyrrol-2-(1H)-yl)-2-(4-fluorophenyl)-3-pyridazin-4-ylimidazo[1,2-b]pyridazine

수율 87.2%

용매

pentanol

반응 조건

후처리

1. 1
   세척the aqueous phase is washed with ethyl acetate
2. 2
   추출the product is extracted with dichloromethane
3. 3
   건조The organic phase is dried over sodium sulfate
4. 4
   농축concentrated under reduced pressure
5. 5
   기타The product is chromatographed on a silica gel column, elution
6. 6
   workup.ADDITIONbeing carried out with a mixture of aqueous ammonia, methanol and dichloromethane (0.2/2/98)

실험 절차

The mixture of 0.90 g (2.8 mmol) of 6-chloro-2-(4-fluorophenyl)-3-(pyridazin-4-yl)-imidazo[1,2-b]pyridazine and 1.7 g (8.3 mmol) of 5-benzyloctahydropyrrolo[3,4-c]pyrrole in 15 ml of pentanol is heated in a sealed tube at 150° C. for 18 hours. The reaction medium is poured into a 1N aqueous solution of hydrochloric acid and the aqueous phase is washed with ethyl acetate. The aqueous phase is then basified using aqueous sodium hydroxide and the product is extracted with dichloromethane. The organic phase is dried over sodium sulfate and then concentrated under reduced pressure. The product is chromatographed on a silica gel column, elution being carried out with a mixture of aqueous ammonia, methanol and dichloromethane (0.2/2/98), to give 1.2 g of solid in the form of an amorphous white foam.

출처