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三光气法合成2,6-二氟苯甲酰基异氰酸酯

Synthesis of 2,6-difluorobenzoyl isocyanate by triphosgene method

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2,6-二氟苯甲酰基异氰酸酯(DFBI)是合成苯甲酰脲类杀虫剂的重要中间体,使用光气合成DFBI的工艺危险性很大,使用草酰氯的合成工艺成本较高.三光气(BTC)是剧毒的光气和双光气的绿色替代品,不仅毒性低、使用安全方便,而且反应条件温和、计量准确、价格低廉.采用BTC与2,6-二氟苯甲酰胺(FBA)反应合成DFBI,研究了单一因素对合成DFBI的影响.实验结果表明,以氯苯为溶剂,投料n(BTC)∶n(FBA)=1.0∶1.5,BTC分2次均等投料,第1阶段冷光气化-5℃反应1 h,第2阶段热光气化126~128℃反应4 h的较适宜条件下,产品收率达到86.4%.BTC可以较稳定、安全地使用,易于工业化.
2,6-Difluorobenzoyl isocyanate(DFBI)is an important intermediate for the synthesis of ben-zoyl urea pesticides.The synthetic process of DFBI with phosgene is very dangerous,and the cost of preparation of DFBI using oxalyl chloride is high.Bis(trichloromethyl)carbonate(BTC)is a green sub-stitute for the highly toxic phosgene and diphosgene.It not only is low in toxicity,safe and convenient to use,but also has mild reaction conditions,accurate measurement and low price.The DFBI was synthe-sized by the reaction of BTC with 2,6-difluorobenzamide(FBA),and the effect of single factor on the synthesis of DFBI was studied.The experimental results show that the optimal conditions are as follows:Chlorobenzene is used as the solvent,the molar ratio of feeding is n(BTC)∶n(FBA)=1.0∶1.5,BTC is equally fed in two times,and the first stage of cold-phosgenation is reacted at-5 ℃ for 1 h,the second stage of thermal-phosgenation is reacted at 126-128 ℃ for 4 h,and the product yield could reach 86.4%.BTC can be used stably and safely,and the process is easy to industrialize.

triphosgene2,6-difluorobenzamidedifluorobenzoyl isocyanatechlorobenzene

张天永、鞠雯超、姜爽、李彬、刘余峰、张朋飞

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天津大学化工学院,天津市应用催化科学与工程重点实验室,天津 300354

天津化学化工协同创新中心,天津 300072

天津市功能精细化学品技术工程中心,天津 300354

河北君瑞沣新材料有限公司,河北衡水 053010

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三光气 2,6-二氟苯甲酰胺 二氟苯甲酰异氰酸酯 氯苯

2024

化学工业与工程
天津化工学会 天津大学

化学工业与工程

CSTPCD北大核心
影响因子:0.406
ISSN:1004-9533
年,卷(期):2024.41(4)
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