Sulfuric Acid → HCID 547246, compound

Participants

Reaction Steps

A mixture of 8 g. (0.027 mole) of 10-(2-dimethylaminoethyl)-10,11-dihydro-5-methyl-5H-dibenzo[a,d]cyclohepten-5-ol and 250 ml. 2M-sulfuric acid is refluxed for 2 hours. The mixture is cooled in ice and made basic by the addition of solid potassium hydroxide. The mixture is extraced with methylene chloride. The methylene chloride is washed with water, dried over anhydrous magnesium sulfate and evapored in vacuo. The oily residue is distilled at 140° C/0.5 mm and the distillate is dissolved in ethanol. The resulting precipitate is filtered and recrystallized from diethylether-ethanol 1:1 to give the product 10-(2-dimethylaminoethyl)-10,11-dihydro-5-methylene-5H-dibenzo[a,d]cycloheptene, m.p. 171° to 172 C.

Provenance & Evidence