Synthesis Of 1,3-Dimethyl-butylamine Citrate

1,3-Dimethyl-butylamine citrate can be applied in the fields of pharmaceuticals and fine organic chemistry as intermediate or catalyst.In recent years,because of the similarity excitation effect with 1,3-dimethyl-amylamine for human,1,3-dimethyl-butylamine has also been studied to use as the succedaneum of1,3-dimethyl-amylamine in the health care products.The efficacy of1,3-dimethyl-butylamine citrate is mainly reflected in increasing energy,enhancing spiritual,improving the body energy,especially in cloric restriction or energy concentration for athlete.While being used in diet products for weight control,it can significantly reduce appetite and inhibit the heat effect.In the work,1,3-dimethyl-butylamine citrate was synthesized through two different routes from methyl isobutyl ketone as starting material.The first route underwent oximation reaction in which the starting material was transferred to methyl isobutyl ketone oxime(1)and then atmospheric pressure reduction of the intermediate 1 to afford1,3-dimethyl-butylamine(2).In the second route,methyl isobutyl ketone reacted with ammonia under high pressure catalyzed hydrogenation to give 1,3-dimethyl-butylamine(2).The prepared intermediate 2 reacts with citric acid to give the final product1,3-dimethyl-butylamine citrate.In the paper,two routes were researched in detail and the optimal condition was presented respectively,which laid a solid theoretical foundation for commercial process of 1,3-dimethyl-butylamine citrate.The synthetic product 1,3-dimethyl-butylamine citrate and the main intermediate 2were characterized by FT-IR,DSC-TGA,LC-MS and ~1H NMR.While the relevant gas chromatograph(GC)analysis method for the main intermediate 1,3-dimethyl-butylamine(2)was determined and validation,which provided a important monitoring means for detection and industrial production of intermediate.