Catalytic Synthesis Of The α-multi-branched-chain Acidamide Under The Mild Conditions

The a-multi-branched-chain acidamide are importantly organic materials and intermediates for the synthesis of pharmaceuticals, pesticides, surfactants and extractants. In this paper, the main aim is to study the reaction of tert-butyl alcohol and different amines by access to a large number of papers and the analysis on the synthetic routes of the primary amines. Through the selection of suitable heteropoly acid catalyst and finding the right technological conditions of the amination reaction of tert-bntyl alcohol to provide the necessary experimental data for industrial production of the amination.First of all, using the phosphotungstic acid to catalyze the reaction of tert-butanol and p-toluene sulfonamide that is to systhesis N-tertbutylp-toluene sulfonamide. Through the orthogonal experiment, getting the initially optimal conditions. One by one investigating solvent, time, temperature, amount of catalyst on impacting the yield. The optimum conditions are as follows:formic acid as the solvent, temperature at70℃, reaction time6h, catalyst usage for the15%quality of p-toluenesulfonamide, alcohol amine ratio is10:1, N-tertbutylp-toluene sulfonamide’s yield up to95%.Secondly, supported phosphotungstic acid catalyzes the reaction of tert-butanol and urea. Using the orthogonal experiment to select the optimal conditions, and then individually inspecting the effect of solvent, temperature, time, material ratio and the amount of catalyst on the synthesis of tert-Butyl urea. The most suitable reaction conditions:(1) temperature: amination temperature of75℃;(2) the reaction time was25h (the longer, the production rate is relatively higher);(3)(n)tert-butyl alcohol:(n) urea is4:1;(4) the amount of catalyst is30%of urea. Under these conditions, N-tert-Butyl urea production rate is27.5%. In addition, formic acid is best solvent. However, if taking into account the economic benefits, the reaction time to select20h, without solvent the materials ratio of4:1. Repeatability of catalyst is fine after using10times. At the same time to explore the reaction mechanism. The process has overcome the problems of concentrated sulfuric acid to catalyze the synthesis of tert-Butylurea process with high yield and almost no waste emissions, environmental-friendly characteristic, and is suitable for industrialization.