반응 #41236

반응 방정식

L-tartaric acid

product

2-[4′-(3aR,6aR)-(5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl)-1,1′-biphenyl-4-yl]pyridazin-3(2H)-one

→

title compound

수율 94.8%

2-[4′-(3aR,6aR)-(5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl)-1,1′-biphenyl-4-yl]pyridazin-3(2H)-one L-tartrate

수율 94.8%

용매

water

ethanol

반응 조건

후처리

1. 1
   온도The mixture was heated
2. 2
   온도under reflux and after 30 minutes most solids
3. 3
   workup.DISSOLUTIONhad dissolved
4. 4
   온도The mixture was cooled at 5° C. per hour to 60° C.
5. 5
   온도After cooling the mixture to −15° C. the product slurry
6. 6
   여과was filtered
7. 7
   기타dried at 45-50° C. overnight

실험 절차

A solution of 3.45 g of L-tartaric acid (1.07 eq.) in 56 g of water was added to a flask containing a slurry of 8.00 g of the product of Example 41G in anhydrous ethanol (44 g). The mixture was heated under reflux and after 30 minutes most solids had dissolved. The mixture was cooled at 5° C. per hour to 60° C., and then allowed to cool to ambient temperature overnight. After cooling the mixture to −15° C. the product slurry was filtered and dried at 45-50° C. overnight to provide the title compound (10.64 g, 94.8%).

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