摘要
4-叔丁氧基苯乙烯(PTBS)是合成KrF光刻胶成膜树脂的重要单体之一。以4-溴苯酚和异丁烯为起始原料,经酸催化得1-溴-4-叔丁氧基苯,再制备其格氏试剂,与氯乙烯发生Kumada偶联反应得目标化合物4-叔丁氧基苯乙烯。考察了催化剂类型、添加量及反应温度等对产物收率的影响。结果显示,浓硫酸催化制备的中间体收率为96.5%;三溴化铁催化偶联反应得到的目标化合物收率达90.5%;产物纯度均大于99.5%。通过核磁共振测试,中间体及目标产物的分子结构得到了表征。
4-tert-butoxystyrene(PTBS)is one of the important monomers for the film-forming resin of KrF photoresist.4-Bromophenol and isobutylene were used as the starting materials.Under acid catalysis,1-bromo-4-tert-butoxybenzene was obtained.Then its Grignard reagent was prepared and underwent Kumada coupling reaction with vinyl chloride to obtain the target compound,4-tert-butoxystyrene.The effects of the cata-lyst type,dosage,and reaction temperature on the product yield were explored.The results show that:The intermediate was prepared via catalysis by concentrated sulfuric acid with a yield of 96.5%;The coupling reaction catalyzed by iron tribromide afforded the target compound with a yield of 90.5%;The purity of the product was greater than 99.5%.Through nuclear magnetic resonance testing,the molec ular structures of the intermediate and the target product were characterized.
作者
卢畅吟
韦尚徐
覃秀灵
覃洁容
吴忠联
姚志艺
Lu Changyin;Wei Shangxu;Qin Xiuling;Qin Jierong;Wu Zhonglian;Yao Zhiyi(Guigang Weixin Technology Co.,Ltd.,Guangxi,537124;Guigang Dingyuan Synthetic Materials Manufacturing Co.,Ltd.,Guangxi,537124;School of Chemistry and Chemical Engineering,Jiangsu University of Technology,Jiangsu,213001)
出处
《当代化工研究》
2025年第9期170-172,共3页
Modern Chemical Research
基金
2024年自治区统筹支持工业振兴基金“制造业创新成果大规模工业化应用”资助项目“高端肉桂酸系列产品(光刻胶树脂及高纯溶剂)项目”
中央引导地方科技发展资金资助项目“半导体关键材料——光刻树脂及单体产业化项目”(项目编号:贵科中引专项2022)。
