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该文以苯肼、环己酮为起始原料,经醋酸环化合成四氢咔唑,收率达70.5%,再与溴乙烷经烷基化反应制得9-乙基四氢咔唑。产物的结构经~1HNMR和~(13)CNMR表征。经单因素实验考察,确定合成9-乙基四氢咔唑的最优条件为:n(四氢咔唑)∶n(溴乙烷)∶n(氢氧化钠)=1∶4∶1.5,m(四氢咔唑)∶m(碘化钾)=1∶0.01,c(四氢咔唑)=0.50 mol/L,c(十六烷基三甲基溴化铵)=2.5×10~(-3)mol/L,乙腈为溶剂,回流反应9 h,收率为86.0%。该路线与传统工艺(环己酮先经氯化再与N-乙基苯胺缩合)相比,可避免氯化副产物生成,反应易控制,更适合工业生产。
In this paper, phenylhydrazine, cyclohexanone as the starting material, acetic acid cyclization synthesis of tetrahydrocarbazole, the yield was 70.5%, and then with ethyl bromide by alkylation 9-ethyl tetrahydrocarbazole . The structure of the product was characterized by ~ 1HNMR and ~ (13) CNMR. The optimum conditions for the synthesis of 9-ethyltetrahydrocarbazole were confirmed as follows: n (tetrahydrocarbazole) :n (bromoethane) :n (sodium hydroxide) = 1: 4: 1.5, m (tetrahydrocarbazole): m (potassium iodide) = 1: 0.01 c (tetrahydrocarbazole) = 0.50 mol / L c = cetyltrimethylammonium bromide = 2.5 × 10 ~ 3) mol / L, acetonitrile as solvent, refluxed for 9 h, the yield was 86.0%. Compared with the traditional process (cyclohexanone chlorination first and N-ethyl aniline condensation), the route can avoid the formation of chlorinated by-products and the reaction is easy to control and more suitable for industrial production.