Study on by-products and synthesis of 4-ethoxy-2,3-difluorophenylacetic acid
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    Abstract:

    Abstract:More than 99% purity of liquid crystal intermediate of 4-ethoxy-2,3-difluorophenyl acetic acid was synthesized via alkaline hydrolysis and acidification after Willgerodt-Kindler reaction with 4-ethoxy-2,3-difluoroacetophenone as the starting material. The target compound was characterized by 1HNMR、IR and GC-MS. The results of condition experiments showed the effect of Willgerodt-Kindler reaction was best when the molar ratio of 4-ethoxy-2,3-difluoroacetophenone/sulfur/morpholine was 1:2:4, the reaction temperature was 105~115 ℃ and the reaction time was 2 h.The mass ratio of the main product was 71.54%,the mass ratio of the by-product of 4-ethoxy-2-morpholine-3-fluoro-phenyl thiomorpholine amide was 14.60%.The generation reason of the by-product during Willgerodt-Kindler reaction was proposed according to the results of experiments,and its structure was confirmed by 1HNMR and GC-MS.

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History
  • Received:January 21,2013
  • Revised:March 20,2013
  • Adopted:April 03,2013
  • Online: May 30,2013
  • Published:
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