Reaction #41264

Reaction equation

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

Solvents

water

—

solution

Conditions

Workup

1. 1
   Otherwas prepared
2. 2
   Otheryielding a clear solution
3. 3
   FiltrationThe solution was then filtered
4. 4
   Temperaturethe supernatant cooled to ambient temperatures naturally overnight
5. 5
   OtherThe solids precipitated over the night
6. 6
   workup.DISSOLUTIONwere dissolved again the next day
7. 7
   Temperatureby heating the suspension to about 90° C
8. 8
   TemperatureThe solution was cooled slowly

Procedure

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