摘要
以苯酚为原料,经取代、环合、溴代和氯磺化4步反应合成了含有二氢苯并呋喃骨架的杂环类磺酰氯衍生物5-溴-2,3-二氢苯并呋喃-7-磺酰氯.针对氯磺化步骤优化了工艺条件.优化条件为:n(5-溴-2,3-二氢苯并呋喃)∶n(氯磺酸)=1∶6、反应温度25℃、反应时间2.5 h.优化条件下目标产物收率达81％,其结构经1HNMR、13CNMR、质谱和IR确证.
Abstract
5-Bromo-2,3-dihydrobenzofuran-7-sulfonyl chloride as a derivative of heterocyclic sulfonyl chloride containing a dihydrobenzofuran skeleton was synthesized from phenol through a four-step reaction including substitution,cyclization,bromination and chlorosulfonation.The synthetic conditions were optimized for the chlorosulfonation step.The optimized conditions were as follows:the molar ratio of n(5-bromo-2,3-dihydrobenzofuran)∶n(chlorosulfonic acid)=1∶6,under the reaction temperature of 25℃,reaction time of 2.5 h.The yield under the optimized conditions reached 81％.The target product was confirmed by 1H NMR,13C NMR,HRMS,and IR.
基金项目
江苏省高等学校"青蓝工程"项目(苏教师函[2023]27号)
苏州市科技计划基础研究计划(SKY2023135)
苏州卫生职业技术学院科技创新团队项目(SZWZYTD202204)
维普
万方数据