Acetone → HCID 86587370, compound

Temperature

60 °C

A 2 L 4-neck flask was charged with O-desmethyl-venlafaxine (75.0 g, 0.285 mol), acetone (627 mL), succinic acid (34.50 g, 0.29 mol), and water (197.5 mL). The suspension was warmed to 60° C. and filtered through a pad of Celite. The filter pad was washed with a warm mixture of acetone (97 mL) and water (30.6 mL). The filtrate was transferred to a clean 2 L flask rinsing with acetone (50 mL). The temperature of the solution was 28° C. The solution was allowed to cool and crystallization began at 23° C. The mixture was then rapidly cooled in an ice/water bath to 0-5° C. The mixture was stirred at 0-5° C. for 2 hours. The solids were isolated by filtration and washed with cold aqueous acetone (2×200 mL, 25:75 v/v water/acetone). The wet filter cake was dried in a vacuum oven at 35±5° C. (50 mm Hg) for 48 hours to yield ODV succinate monohydrate as white crystals (89.5 g, 78.7%).

1. filtrationfiltered through a pad of Celite
2. washThe filter pad was washed with a warm mixture of acetone (97 mL) and water (30.6 mL)
3. customThe filtrate was transferred to a clean 2 L flask
4. washrinsing with acetone (50 mL)
5. customwas 28° C
6. temperatureto cool
7. customcrystallization
8. custombegan at 23° C
9. temperatureThe mixture was then rapidly cooled in an ice/water bath to 0-5° C
10. customThe solids were isolated by filtration
11. washwashed with cold aqueous acetone (2×200 mL, 25:75 v/v water/acetone)
12. customThe wet filter cake was dried in a vacuum oven at 35±5° C. (50 mm Hg) for 48 hours

ORD record

ord-e144a7ed154e4b6dbb0159707d2354ed

Source dataset

uspto-grants-2004_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06673838B2