| 微波辐射及聚乙二醇-600催化条件下无溶剂法制备柠檬腈 |
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| 引用本文： | 黄祖良,陆海峰,韦国锋,黄徽,韦柳斌.微波辐射及聚乙二醇-600催化条件下无溶剂法制备柠檬腈[J].精细化工,2008,25(6):576-579. |
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| 作者姓名： | 黄祖良 陆海峰 韦国锋 黄徽 韦柳斌 |
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| 作者单位： | 右江民族医学院,化学教研室,广西,百色,533000;广西万山香料有限公司,广西,灵山,535400 |
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| 摘 要： | 以柠檬醛为原料,在微波辐射及相转移催化剂聚乙二醇-600催化作用下,由SiO2/Na2CO3-NaOH混合碱促进的无溶剂一步法直接制备柠檬腈。确定的最佳反应条件是:n(柠檬醛)∶n(盐酸羟胺)=1∶(1.6~1.8);对应每mmol柠檬醛,SiO2的用量为0.20~0.25 g;催化剂为m(PEG-600)/m(柠檬醛)=0.08,磨细后用功率为520W的微波辐射,反应4 min。在此条件下,从柠檬醛制备柠檬腈的平均产率达90.7%。
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| 关 键 词： | 柠檬腈 无溶剂 微波辐射 聚乙二醇-600 香料与香精 |
| 文章编号： | 1003-5214(2008)06-0576-04 |
| 修稿时间： | 2007年12月14 |
Synthesis of Lemonile from Citral Under Microwave Assisted Solvent-free Condition with Phase Transfer Catalysis of Polyethylene Glycol 600 |
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| HUANG Zu-liang,LU Hai-feng,WEI Guo-feng,HUANG Hui,WEI Liu-bin.Synthesis of Lemonile from Citral Under Microwave Assisted Solvent-free Condition with Phase Transfer Catalysis of Polyethylene Glycol 600[J].Fine Chemicals,2008,25(6):576-579. |
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| Authors: | HUANG Zu-liang LU Hai-feng WEI Guo-feng HUANG Hui WEI Liu-bin |
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| Abstract: | Under microwave irradiation and phase transfer catalysis of polyethylene glycol 600,lemonile was prepared directly from citral/NH2OH·HCl in the presence of SiO2/Na2CO3-NaOH under solvent-free condition in one step.The optimal reaction conditions were:n(citral)∶n(hydroxylamine hydrochloride)=1∶(1.6～1.8),the dosage of SiO2 0.25～0.3 g/mmol citral,using PEG-600 as catalyst,m(polyethylene glycol 600)/m(citral)=0.08,grinding thoroughly and heating by microwave of 520 W power about 4 minutes.Under these conditions,the average yield of lemonile from citral was up to 90.7%. |
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| Keywords: | lemonile solvent-free microwave irradiation polyethylene glycol 600 perfumes and essences |
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