Reaction of 3-[1-(dimethylamino)ethyl]phenol (I) with N-ethyl-N-methylcarbamoyl chloride (II) and sodium hydride in tetrahydrofuran gives racemic N-ethyl-N-methylcarbamic acid 3-[1-(dimethylamino)ethyl]phenyl ester (III), which is resolved by recrystallization with (+)-D-di-O,O'-(p-toluoyl)tartaric acid in methanol followed by treatment with base.