| 1-苯乙烯基膦酸的合成工艺改进 |
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| 引用本文： | 龚必伟,傅相锴,申红胜,马丽华,夏永建. 1-苯乙烯基膦酸的合成工艺改进[J]. 精细化工, 2008, 25(6): 603-605 |
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| 作者姓名： | 龚必伟 傅相锴 申红胜 马丽华 夏永建 |
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| 作者单位： | 西南大学,化学化工学院,西南大学应用化学研究所,重庆市应用化学重点实验室,重庆,400715;西南大学,化学化工学院,西南大学应用化学研究所,重庆市应用化学重点实验室,重庆,400715;西南大学,化学化工学院,西南大学应用化学研究所,重庆市应用化学重点实验室,重庆,400715;西南大学,化学化工学院,西南大学应用化学研究所,重庆市应用化学重点实验室,重庆,400715;西南大学,化学化工学院,西南大学应用化学研究所,重庆市应用化学重点实验室,重庆,400715 |
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| 摘 要： | 以苯乙酮(AP),三氯化磷(PT)和冰醋酸(AA)为原料,合成了1-苯乙烯基膦酸。考察了原料配比、第一步反应温度和时间对产物收率的影响,优化的工艺条件为:n(AP)∶n(PT)∶n(AA)=1∶1.5∶3.5,反应温度20℃,反应时间6 h,加冰醋酸搅拌过夜,直接加入浓盐酸后回流5 h,冷却,二次重结晶,所得1-苯乙烯基膦酸产物经1HNMR,31PNMR,FTIR和熔点测定进行确认。与文献方法相比,该文报道的工艺缩短了反应步骤,收率从83%提高到90%。
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| 关 键 词： | 苯乙酮 三氯化磷 冰醋酸 1-苯乙烯基膦酸 精细化工中间体 |
| 文章编号： | 1003-5214(2008)06-0603-03 |
| 修稿时间： | 2007-12-01 |
Improvement in Synthesis Method of 1-Phenylvinylphosphonic Acid |
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| GONG Bi-wei,FU Xiang-kai,SHEN Hong-sheng,MA Li-hua,XIA Yong-jian. Improvement in Synthesis Method of 1-Phenylvinylphosphonic Acid[J]. Fine Chemicals, 2008, 25(6): 603-605 |
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| Authors: | GONG Bi-wei FU Xiang-kai SHEN Hong-sheng MA Li-hua XIA Yong-jian |
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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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| Keywords: | acetophenone phosphorus trichloride acetic acid 1-phenylvinylphosphonic acid fine chemical intermediates |
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