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Facile Synthesis of (3, 3-Difluorcyclohexyl)Methanmine |
ZHAO Yu-ling, QIU Ji-kuan |
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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Received: 12 November 2014
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