Study On The Synthesis Of The 4-tert-butylcatechol

With the rapid development of Petro-chemical technology and macromolecule materials industry, the using area of 4-tert-butylcatechol is expanded endless, the amounts of usage becomes great, the demand of product quality becomes higher. Thus, it becomes significant to develop new technology of 4-tert-butylcatechol and to improve the domestic technology and satisfy the domestic demand of the products.The research on the synthesis of 4-tert-butylcatechol, alkylation of catechol had higher economic importance. Three steps were applied to synthesize 4-tert-butylcatechol. First, o-ethoxyphenol was prepared from o-chlorophenol, which is the key step. Second, catechol was prepared from o-ethoxyphenol. Third, 4-tert-butylcatechol was prepared.O-ethoxyphenol was prepared by phase-transfer catalytic reaction under microwave irradiation from o-chlorophenol. Intellective microwave reactor,commercial microwave reactor and high efficiency microwave reactor were used, The effect of reaction time,reaction temperature,microwave power,raw material ratio,catalyst and solvent on reaction result were studied. The results were dissculed and analysed. Catechol was prepared from o-ethoxyphenol at the presence of sodium amide, The effect of process reaction time,reaction temperature,raw material ratio and method of additive materials on reaction result was studied. 4-tert-butylcatechol was prepared from the reaction of catechol and alkylation reagent methyl tert-butyl ether, The effect of reaction time,reaction temperature,raw material ratio,catalyst and method of additive materials on reaction result was studied. A suit of method for middle-cntrolled analysis which was associatived with extraction and GC was established, products were token by melting point,IR and MS.At the effection of sodium amide, o-ethoxyphenol was cleaved with tetralin as solvent, then acidified to catechol. By optimizing the experiment conditions, the optimum conditions was gained, when o-ethoxyphenol:sodium amide = 1:2.1(mol), reaction temperature was 200℃, reaction time was 6h, the yield of catechol was 89.00%. With methyl tert-butyl ether as a tert-butyl solvent, a tert-butyl was added tert-butyl onto catechol. The optimum experimental conditions was gained by making the orthogonal experiment, reaction temperature was 110℃,reaction time was 2.5h, catechol:MTBE=1:1.5(mol),H2SO4 was 1.225g, the yield of 4-tert-butylcatechol was 72.26%.