The Synthesis Of Benzenesulfonyl Chloride M-methoxy

Organic intermediate is an important fine chemical substance, the technology of benzenesulfonyl chloride m-methoxy, used to make dyestuff and medicine intermediate composition, is complex and less yield, which have restricted it's apply and development further.This paper has studied on the synthesis of benzenesulfonyl chloride m-methoxy, through diazotization, hydrolysis, methylation and chlorosulfonat-ion process, m-aminobenzenesulfonic acid as raw material. In the optimal condition, the total yield attends to 74.27%, the purity is 98.02%, and the pure yield is 72.83%, compared with the literature value, the yield increases 24.44%.In the paper, by the means of orthogonality experiment and factor checking, the optimal technical conditions of benzenesulfonyl chloride m-methoxy are as follows: the usage of vitriol: m-aminobenzenesulfonic acid is 3.0:1 (mol ratio), the usage of sodium nitrite : m-aminobenzenesulfonic acid is 1.05:1 (mol ratio), reactive temperature is 9, reactive time is 2hours, the concentration of diazotization vitriol is 75%(wt%); hydrolysis temperature is 90 , the concentration of diluted vitriol is 10% and the hydrolysis time is 1hour; during the course of methylation, the usage of dimethyl sulfate is 1.00(mol ratio), the usage of sodium hydroxide is 1.20(mol ratio), methylation temperature is 85癈, the reactive time is Shours; during the chlorosulfonation, the usage of chrolosul hanic acid is 6.0(mol ratio), the usage of thoinly chloride is 3.0(mol ratio), reactive temperature is 75 , reactive time is Shours, the hydrolysis temperature is 5, and the concentration of diazotization vitriol is 75%(wt%).The methods of chemical analysis of m-Hydroxybenzenesulfonic sodium, m-methyoxybenzenesulfonic sodium, the benzenesulfonyl chloride m-methoxy, have been established.