| 3,3-二氟环己基甲胺的简便合成 |
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| 引用本文： | 赵玉灵,仇记宽. 3,3-二氟环己基甲胺的简便合成[J]. 合成化学, 2015, 23(10): 971-973. DOI: 10.15952/j.cnki.cjsc.1005-1511.2015.10.0971 |
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| 作者姓名： | 赵玉灵 仇记宽 |
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| 作者单位： | 河南师范大学 化学化工学院 精细化学品绿色制造河南省协同创新中心，河南 新乡 453007 |
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| 基金项目： | 国家自然科学基金资助项目（21403060）； 河南省教育厅科学技术研究重点项目（14A150039， 14A150038） |
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| 摘 要： | 以环己烯酮和硝基乙酸乙酯为原料，经Michael加成、水解脱羧、亲核氟化和还原反应合成了3,3-二氟环己基甲胺(4)，总收率55％，其结构经1H NMR和MS确证。在最佳还原反应条件［1,1-二氟-3-硝甲基环己烷83.73 mmol, Raney Ni (80％)和NH3·H2O为共催化剂，EtOH为溶剂，于室温反应12 h］下，4的收率82%。
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| 关 键 词： | 环己烯酮 3 3-二氟环己基甲胺 合成 |
| 收稿时间： | 2014-11-12 |
Facile Synthesis of (3, 3-Difluorcyclohexyl) Methanmine |
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| ZHAO Yu-ling,QIU Ji-kuan. Facile Synthesis of (3, 3-Difluorcyclohexyl) Methanmine[J]. Chinese Journal of Synthetic Chemistry, 2015, 23(10): 971-973. DOI: 10.15952/j.cnki.cjsc.1005-1511.2015.10.0971 |
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| Authors: | ZHAO Yu-ling QIU Ji-kuan |
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| Affiliation: | Collaborative Innovation Center of Henan Province for Green Manufacturing of Fine Chemicals, School of Chemistry and Chemical Engineering, Henan Normal University, Xinxiang 453007, China |
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| Abstract: | (3,3-Difluorcyclohexyl)methanmine（4） in total yield of 55% was synthesized by Michael addition reaction, hydrolyzation decarboxylation, nucleophilic fluorination and reduction reaction， usingcyclohex-2-en-1-one and ethyl nitroacetate as raw materials. The structure was confirmed by 1H NMR and MS. Under the optimal reaction conditions［1，1-difluoro-3-(nitromethyl)cyclohexane 83.73 mmol, Raney Ni(80％)+NH3·H2O as the co-catalyst, EtOH as the solvent, at room temperature for 12 h］, the yield of 4 was 82%. |
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| Keywords: | cyclohex-2-en-1-one 3 3-difluorcyclohexylmethanmine synthesis |
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