Citric Acid → HCID 86751488, compound

Participants

Reaction Steps

Combine (E)-1-[4-(4-diethylaminobutoxy)phenyl]-1,2-diphenyl-2-chloro-ethylene hydrochloride salt (138.4 g, 0.294 mol) and dichloromethane. Add with stirring a solution of sodium hydroxide (12.8 g) in water (100 mL). After 30 minutes, separate the layers and extract the aqueous layer with dichloromethane. Dry the combined organic layers over MgSO4, filter, and evaporate in vacuo to give a residue. Combine the residue and acetone (1 L). Filter and combine the filtrate with a solution of citric acid (56.5 g, 0.294 mol) in acetone (2 L). Allow to stand at ambient temperature to give a solid. Collect the solid by filtration, rinse with acetone, and dry to give the title compound as a solid: mp; 133°-135° C.

Provenance & Evidence