反応 #41236

反応方程式

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

収率 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

収率 94.8%

溶媒

water

ethanol

反応条件

後処理

1. 1
   温度The mixture was heated
2. 2
   温度under reflux and after 30 minutes most solids
3. 3
   workup.DISSOLUTIONhad dissolved
4. 4
   温度The mixture was cooled at 5° C. per hour to 60° C.
5. 5
   温度After cooling the mixture to −15° C. the product slurry
6. 6
   ろ過was filtered
7. 7
   その他dried at 45-50° C. overnight

実験手順

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%).

出典