摘要
选择二卤代苯的间接巯基化法,以甲硫醇钠与邻二氯苯为原料在二甲基甲酰胺溶剂中反应制得邻苯二甲硫酚,再经酸性条件下水解得目标化合物,优化工艺条件为:n(邻二氯苯)∶n(甲硫醇钠)=1∶5,分段升温90~100℃,120~130℃,收率达93%,适合工业化生产。
1,2-Benzenedithiol was synthesized by the reaction of methyl mercaptan sodium with o-dichlorobenzene in DMF followed by acidic hydrolysis,and the route was optimized for industrial production.Optimal conditions were obtained that molar ratio of o-dichlorobenzene to methyl mercaptan sodium was 1 to 5 and the temperature was controlled in 2 steps of 90~100℃ and 120~130℃.The yield of 1,2-benzenedithiol reached to 93%.
出处
《精细化工中间体》
CAS
2010年第6期43-44,55,共3页
Fine Chemical Intermediates
基金
杭州市属高校绿色精细化工研究与技术转化重点实验室开放基金项目(KFJ200902)
关键词
苯二硫酚
甲硫醇
巯基化
水解
合成
benzenedithiol
methyl mercaptan
sulfhydryl
hydrolysis
synthesis