Réaction #41264

Équation de réaction

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

dichloromethane

→

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

Solvants

water

—

solution

Conditions de réaction

Traitement

1. 1
   Autrewas prepared
2. 2
   Autreyielding a clear solution
3. 3
   FiltrationThe solution was then filtered
4. 4
   Températurethe supernatant cooled to ambient temperatures naturally overnight
5. 5
   AutreThe solids precipitated over the night
6. 6
   workup.DISSOLUTIONwere dissolved again the next day
7. 7
   Températureby heating the suspension to about 90° C
8. 8
   TempératureThe solution was cooled slowly

Mode opératoire

2-{4′-[(3aR,6aR)-5-Methylhexahydropyrrolo[3,4-b]pyrrol-1(2H)-yl]-1,1′-biphenyl-4-yl}pyridazin-3(2H)-one tartrate (Form A) was suspended in 1 mL of solution mixture, which was prepared by mixing 5.0 mL of dichloromethane with 5.0 mL of 20% water (in methanol). The suspension was vortexed and heated to about 48° C. yielding a clear solution. The solution was then filtered and the supernatant cooled to ambient temperatures naturally overnight. The solids precipitated over the night were dissolved again the next day by heating the suspension to about 90° C. The solution was cooled slowly by progressively lowering the temperature of the water bath to ambient temperatures. Single crystals were offered.

Source