Chen Xing-quan, Z. Cui’e, L. Hong
2005
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Journal
Shaanxi Chemical Industry
Abstract
This paper reports a new process of synthesizing paracetamol from phenol by acetylization,oximation and Beckmann rearrangement.4-hydroxyacetophone(Ⅰ) is prepared by reaction of phenol and acetic anhydride in the presence of HF catalyst at 80℃ for 1h.4-hydroxyacetophenone oxime(Ⅱ) is produced by the oximation of(Ⅰ) extracted by acetic ester and hydroxylamine sulfate in buffer solution(pH = 3~7) at 101~102℃ for 1h.The rearrangement of(Ⅱ) in the presence of SOCl_2 catalyst and acetic ester solvent can gets the title product,which is purified and decolorized in the presence of activated C processed by hydrochloric acid in water.In order to prevent by-product,a little KI is added in the rearrangement.The total yield is 60%,the purity of the product is over 99.9%(HPLC) and melting point is 170~172℃.