摘要
提出了一种合成6-溴-4,4-二氢苯并噻喃的新路线,并对合成过程中的工艺条件进行了优化,得到了较优的反应条件.本工艺以溴苯为起始原料,经氯磺化、还原、硫醚化、环合4步反应得到6-溴-4,4-二氢苯并噻喃,最终收率为88.5%.除还原这一步需要较高温度外,其他3步反应均在50℃以下进行,既降低了能耗,又减少了副产物的生成.与已有工艺路线相比,本工艺路线具有成本低廉的优点,适合工业化生产.
A new route for the synthesis of 6-bromo-4,4-dimethylthiochroman was proposed and the optimized conditions for each step were obtained.Bromobenzene was selected as starting material and 6-bromo-4,4-dimethylthiochroman was prepared via chlorosulfonation,reduction,thioetherification and cyclization with the yield of 88.5%.Except the reduction,which had to be performed at a higher temperature,the other three steps proceeded at temperatures lower than 50oC.Thus both the energy cost and byproducts were decreased.Compared to previous routes,the proposed one in this work is advanced for its lower cost and less contamination,so it is suitable to be industrially amplified.
出处
《浙江大学学报（理学版）》
CAS
CSCD
2012年第2期187-189,共3页
Journal of Zhejiang University（Science Edition）
基金
国家自然科学基金资助项目(21076183)
浙江省自然科学基金资助项目(Y4100147)
