Acetone → HCID 86587370, compound

Participants

Reaction Conditions

Reaction Steps

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%).

Provenance & Evidence