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三光气两相法合成2-氧-5-甲基-3-氢-1,3,4-噁二唑的工艺研究
引用本文:王丛文,姚日生,邓胜松,余三喜.三光气两相法合成2-氧-5-甲基-3-氢-1,3,4-噁二唑的工艺研究[J].安徽化工,2010,36(4):25-28.
作者姓名:王丛文  姚日生  邓胜松  余三喜
作者单位:合肥工业大学化工学院,安徽,合肥,230009;合肥工业大学化工学院,安徽,合肥,230009;合肥工业大学化工学院,安徽,合肥,230009;合肥工业大学化工学院,安徽,合肥,230009
摘    要:以三光气为原料,借助油水两相反应体系合成2-氧-5-甲基-3-氢-1,3,4-噁二唑。利用FT-IR、1HNMR和HPLC对产物进行表征,并对合成工艺进行了优化,在碳酸氢钠为缚酸剂,反应温度为20℃,n碳酸氢钠/n乙酰肼为2.2/1,n三光气/n乙酰肼为0.40/1,滴加三光气的条件下,2-氧-5-甲基-3-氢-1,3,4-噁二唑产率达到85.5%。

关 键 词:三光气  两相法  2-氧-5-甲基-3-氢-1  3  4-噁二唑

Research of the Technology of Synthesise 2-oxygen-5-methyl-3-hydrogen-1,3,4-oxadiazole by Two-phase System with Trisphosgene
WANG Cong-wen,YAO Ri-sheng,DENG Sheng-song,YU San-xi.Research of the Technology of Synthesise 2-oxygen-5-methyl-3-hydrogen-1,3,4-oxadiazole by Two-phase System with Trisphosgene[J].Anhui Chemical Industry,2010,36(4):25-28.
Authors:WANG Cong-wen  YAO Ri-sheng  DENG Sheng-song  YU San-xi
Affiliation:WANG Cong-wen,YAO Ri-sheng,DENG Sheng-song,YU San-xi(School of Chemical Technology,Hefei University of Technology,Hefei 230009,China)
Abstract:Synthesized 2-oxygen-5-methyl-3-hydrogen-1,3,4-oxadiazole with trisphosgene by oil-water two-phase reaction system.The product was identified by FT-IR,1HNMR and HPLC,and optimized synthesis technology.Under the reaction condition,which was NaHCO3 as deacid reagent,reaction temperature was 20℃,the n 缚酸剂/n 乙酰肼 was 2.2/1,the n 三光气/n 乙酰肼 was 0.40/1,trisphosgene droprised,the yield of 2-oxygen-5-methyl-3-hydrogen-1,3,4-oxadiazole can up to 85.5%.
Keywords:trisphosgene  two-phase method  2-oxygen-5-methyl-3-hydrogen-1  3  4-oxadiazole
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