合成技术及应用
閤成技術及應用
합성기술급응용
SYNTHETIC TECHNOLOGY AND APPLICATION
2014年
2期
5-10
,共6页
对羟基苯甲酸%4-乙酰氧基苯甲酸%催化%合成
對羥基苯甲痠%4-乙酰氧基苯甲痠%催化%閤成
대간기분갑산%4-을선양기분갑산%최화%합성
p-Hydroxybenzoic acid%p-Acetoxybenzoic acid%catalysis%synthesis
以对羟基苯甲酸(PHB)和乙酸酐(Ac2 O)为原料,醋酸(HAc)为溶剂,考察浓硫酸和杂环化合物催化合成4-乙酰氧基苯甲酸(PABA),反应物配比为羟基苯甲酸∶乙酸酐∶醋酸=1∶1.05∶0.5,确定最佳催化剂加入量、反应时间和反应温度。结果表明,浓硫酸为催化剂时,最佳反应时间2 h,反应温度100℃,催化剂加入量为 PHB质量的4%,产率67%;杂环化合物P为催化剂时,最佳反应温度80℃,反应时间2 h,催化剂加入量为PHB质量的0.3%,产率99.8%。杂环化合物比浓硫酸对 PABA合成有更好的催化活性,反应条件温和,具有较好的工业化应用前景。
以對羥基苯甲痠(PHB)和乙痠酐(Ac2 O)為原料,醋痠(HAc)為溶劑,攷察濃硫痠和雜環化閤物催化閤成4-乙酰氧基苯甲痠(PABA),反應物配比為羥基苯甲痠∶乙痠酐∶醋痠=1∶1.05∶0.5,確定最佳催化劑加入量、反應時間和反應溫度。結果錶明,濃硫痠為催化劑時,最佳反應時間2 h,反應溫度100℃,催化劑加入量為 PHB質量的4%,產率67%;雜環化閤物P為催化劑時,最佳反應溫度80℃,反應時間2 h,催化劑加入量為PHB質量的0.3%,產率99.8%。雜環化閤物比濃硫痠對 PABA閤成有更好的催化活性,反應條件溫和,具有較好的工業化應用前景。
이대간기분갑산(PHB)화을산항(Ac2 O)위원료,작산(HAc)위용제,고찰농류산화잡배화합물최화합성4-을선양기분갑산(PABA),반응물배비위간기분갑산∶을산항∶작산=1∶1.05∶0.5,학정최가최화제가입량、반응시간화반응온도。결과표명,농류산위최화제시,최가반응시간2 h,반응온도100℃,최화제가입량위 PHB질량적4%,산솔67%;잡배화합물P위최화제시,최가반응온도80℃,반응시간2 h,최화제가입량위PHB질량적0.3%,산솔99.8%。잡배화합물비농류산대 PABA합성유경호적최화활성,반응조건온화,구유교호적공업화응용전경。
In this paper the efficiency of two catalysts,concentrated sulfuric acid and heterocyclic compound P,has been compared during the synthesis of p-Acetoxybenzoic acid (PABA)with p-Hydroxybenzoic acid (PHB) and acetic anhydride as raw materials.Thus the added amount of catalyst,the reaction time and the reaction tem-perature were optimized for the reaction mixture of p-hydroxy benzoic acid,acetic anhydride and acetic acid with a loading ratio of 1∶1∶0.5.It has been found that the most suitable reaction time,reaction temperature,catalyst ad-dition (respect to PHB weight)and productivity of PABA could be 2 h,100 ℃,4%,67% or 2 h,80 ℃, 0.3%,99.8% when using concentrated sulfuric acid or heterocyclic compound P as catalyst,respectively.There-fore,heterocyclic compound P showed a better catalytic activity compared to concentrated sulfuric acid,with which the synthesis of PABA could be carried out under a relatively loose reaction conditions,and promised a great appli-cation foreground.