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4-乙酰氨基环己醇的顺反立体异构化工艺
引用本文:杨能渭,徐正林. 4-乙酰氨基环己醇的顺反立体异构化工艺[J]. 高校化学工程学报, 2002, 16(2): 189-193
作者姓名:杨能渭  徐正林
作者单位:1. 浙江大学化学工程与生物工程学系,浙江,杭州,310027
2. 江苏省建筑科学研究院,江苏,南京,210008
摘    要:以Reney-Ni为催化剂,对4-乙酰氨基环己醇加氢和脱氢反应进行研究,它能促进4-乙酰氨基环己醇立体异构化反应。对反应溶剂,添加剂,H2保护和H2压力等影响因素进行了考察。结果表明:在添加剂AN-1和常压氢保护气氛存在下,以水为溶剂,在回流温度下反应6h,Raney-Ni对顺式反式异构化反应具有较好的效果。反应主要受热力学控制。当以顺反比66:34的4-乙酰氨基环己醇为原料时,平衡产物中,反式异构体可占总醇分离的66%-68%。Raney-Ni在使用过程中,具有良好的催化活性和稳定性。平衡良好的催化活性和稳定性。平衡产物经浓缩结晶,可获得以固体原料计38%以上的较纯(93%)反式异构体。

关 键 词:4-乙酰氨基环己醇 顺反异构化 Raney-Ni 医药中间体
文章编号:1003-9015(2002)02-0189-05
修稿时间:2000-09-15

Cis-trans Epimerizatin Technology of N-(4-hydroxycyclo hexyl) Acetamide
YANG Neng-wei,XU Zheng-lin. Cis-trans Epimerizatin Technology of N-(4-hydroxycyclo hexyl) Acetamide[J]. Journal of Chemical Engineering of Chinese Universities, 2002, 16(2): 189-193
Authors:YANG Neng-wei  XU Zheng-lin
Affiliation:YANG Neng-wei1,XU Zheng-lin2
Abstract:Raney-Ni was adopted as catalyst for dehydrogenation and hydrogenation of N-(4-hydroxycyclohexyl) acetamide, it could improve the cis-trans epimerization of N-(4-hydroxycyclohexyl) acetamide. The effects of solvent, addition agent, H2 protective atmosphere and agent H2 pressure on catalytic reaction were investigated. The study indicate that with addition AN-1 and protective atmosphere of hydrogen, water adopted as solvent, reaction at refluxing temperature in 6h, Raney-Ni appeared to have a fairly good performance for the epimerization of N-(4-hydroxycyclohexyl) acetamide. The major reaction is controlled by thermodynamical equilibrium. When N-(4-hydroxycyclohexyl) acetamide with the cis-trans ratio 66:34 as start material, it can make up 66 to 68 percent trans isomer of total cis and trans isomers in the equilibrium solution through epimerization. Raney-Ni had an excellent catalytic activation and stability in use. By means of concentration and crystallization, an overall yield of more than 38 percent of pure trans isomer (93%) can be obtained from equilibrium products.
Keywords:N-(4-hydroxycyclohexyl) acetamide  cis-trans epimerization  Raney-Ni
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