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Improvement in Synthesis Method of 1-Phenylvinylphosphonic Acid

Xia Yongjian

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Abstract

1-Phenylvinylphosphonic acid was synthesized from acetophenone(AP),phosphorus trichloride(PT),and acetic acid(AA).The optimal reaction conditions were:n(AP)∶n(PT)∶n(AA)=1∶1.5∶5,reaction temperature 20 ℃ and reaction time 6 h.After acetic acid was added,the reaction mixture was stirred over night.Then conc.hydrochloric acid was added,the reaction mixture was refluxed for 5 h,cooled down,and recrystallized to get 1-phenylvinylphosphonic acid.The product was confirmed by 1HNMR,31PNMR,FTIR and melting point.Compared with the literatures,not only the synthesis route is shortened,but also the yield is improved from 83% to 90%.

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What this paper is about

1-Phenylvinylphosphonic acid was synthesized from acetophenone(AP),phosphorus trichloride(PT),and acetic acid(AA).The optimal reaction conditions were:n(AP)∶n(PT)∶n(AA)=1∶1.5∶5,reaction temperature 20 ℃ and reaction time 6 h.After acetic acid was added,the reaction mixture was stirred over night.Then conc.hydrochloric acid was added,the reaction mixture was refluxed for 5 h,cooled down,and recrystallized to get 1-phenylvinylphosphonic acid.The product was confirmed by 1HNMR,31PNMR,FTIR and melting point.Compared with the literatures,not only the synthesis route is shortened,but also the yield is improved from 83% to 90%.

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Available abstract

1-Phenylvinylphosphonic acid was synthesized from acetophenone(AP),phosphorus trichloride(PT),and acetic acid(AA).The optimal reaction conditions were:n(AP)∶n(PT)∶n(AA)=1∶1.5∶5,reaction temperature 20 ℃ and reaction time 6 h.After acetic acid was added,the reaction mixture was stirred over night.Then conc.hydrochloric acid was added,the reaction mixture was refluxed for 5 h,cooled down,and recrystallized to get 1-phenylvinylphosphonic acid.The product was confirmed by 1HNMR,31PNMR,FTIR and melting point.Compared with the literatures,not only the synthesis route is shortened,but also the yield is improved from 83% to 90%.

Key concepts: Acetic acid, Acetophenone, Chemistry, Yield (engineering), Hydrochloric acid, Phosphorus trichloride, Melting point, Nuclear chemistry

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