Manufacturing Process
A 116 parts by weight of phenyl-p-methoxy-chloromethane (4- methoxybenzhydryl chloride) were added to 500 parts by weight of toluene and to the resulting mixture 65 parts by weight of 2-dimethylaminoethanol was added. Then the entire mixture was refluxed for two hours. The refluxed mixture was cooled and 250 parts by weight of a 10% solution of sodium hydroxide were added. This alkaline mixture was then steam distilled until the distillate was only weakly alkaline, for example a pH 7.5-8.
The residue of this steam distillation was then mixed with 200 parts by weight
of benzene and washed with water until the wash waters were practically
neutral. The benzene solution was then evaporated to dryness until the
resulting mixture was of constant weight (145 parts). This product was oily
and was then dissolved in 3000 parts by weight of dry ether; and treated
while being agitated with the theoretically equivalent amount of dry
hydrochloric acid dissolved in ether. This product is an oily product, which
solidified after standing overnight in an ice box. The ether solution was
decanted off and the solidified residue was dissolved in 1500 parts by weight
of dioxane, and then precipitated with 3000 parts by weight of ether while
being continuously agitated. The resulting solid product was the hydrochloride
of 2-(p-methoxy-α-phenylbenzyloxy)-N,N-dimethylethylamine 100 parts by
weight of the desired product were obtained corresponding to a yield of 62%
and having a melting point of 141°C.
