文章摘要
蒋景阳.五环[5.4.0.02,6.03,10.05,9]十一烷-8,11-二酮的还原及试剂的循环使用[J].精细化工,2019,36(11):
五环[5.4.0.02,6.03,10.05,9]十一烷-8,11-二酮的还原及试剂的循环使用
The reduction of pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione and the recycling of the reagent
投稿时间:2019-04-15  修订日期:2019-05-29
DOI:
中文关键词: 五环[5.4.0.02,6.03,10.05,9]十一烷  黄鸣龙还原反应  优化  循环  精细化工中间体
英文关键词: pentacyclo [5.4.0.02,6.03,10.05,9] undecane  Huang Minlon Reduction  optimization  recycle
基金项目:
作者单位E-mail
蒋景阳 大连理工大学 jyjiang@dlut.edu.cn 
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中文摘要:
      以环戊二烯和对苯醌为原料,经过Diels-Alder加成反应、[2 2]光照关环反应、黄明龙还原反应合成五环[5.4.0.02,6.03,10.05,9]十一烷(PCUD)。还原过程中以甲苯和一缩二乙二醇为混合溶剂,采用一锅法在单因素实验的基础上考察了黄鸣龙还原过程中反应温度(T1、T2)和时间(t1、t2)对还原产率的影响。结果表明,在n(五环[5.4.0.02,6.03,10.05,9]十一烷-8,11-二酮):n(KOH):n(水合肼)=1:7.5:14,反应温度T1=120 ℃,T2=180 ℃,反应时间t1=2.5 h,t2=4 h的条件下,五环[5.4.0.02,6.03,10.05,9]十一烷-8,11-二酮的还原收率提高到76.2%。利用PCUD易挥发的特点,考察了其合成的黄鸣龙还原过程中一缩二乙二醇和氢氧化钾的循环使用,在已进行的11次循环中,PCUD的平均收率达到75.2%。
英文摘要:
      The synthesis of pentacyclo [5.4.0.02,6.03,10.05,9] undecane (PCUD) was accomplished by cyclopentadiene and phenylhydrazine as raw materials through Diels-Alder addition reaction, [2 2] cycloaddition reaction, the Huang Minlon Reduction. During the Huang Minlon Reduction, toluene and diethylene glycol as mixed reaction solvents, the effect of reaction temperature (T2) and reaction time (t2) on the reduction yield was investigated by one-pot reaction on the basis of single-factor tests. The optimum conditions were as follows: n(pentacyclo[5.4.0.02,6.03,10.05,9]undecane-8,11-dione):n(potassium hydroxide):n(hydrazine)=1:7.5:14, the reaction being conducted at 120 ℃ for 3 h, followed by react- ion at 180 ?C for 4 h. The reduction yield could reach 76.2%. Subsequently, using the volatile characteristics of PCUD, the recycling of diethylene glycol and potassium hydroxide was investigated in the synthesis process of Huang Minlon Reduction, the average yield of PCUD reached 75.2% in 11 times of recycle that had been carried out.
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