江苏技术师范学院学报
江囌技術師範學院學報
강소기술사범학원학보
JOURNAL OF JIANGSU TEACHERS UNIVERSITY OF TECHNOLOGY
2014年
2期
18-24
,共7页
乙酸苯酯%酯化%4-羟基苯乙酮%Fries重排%4′-羟基查尔酮%羟醛缩合
乙痠苯酯%酯化%4-羥基苯乙酮%Fries重排%4′-羥基查爾酮%羥醛縮閤
을산분지%지화%4-간기분을동%Fries중배%4′-간기사이동%간철축합
phenylacetate%esterification%4′-hydroxyacetophone%Fries rearr -angement reaction%4′-hydroxychalcone%condensation
以苯酚和乙酸酐为原料，经酚酯化反应、Fries重排反应、羟醛缩合来合成4′-羟基查尔酮。对反应的主要因素进行了研究，结果表明：酚酯化反应的温度应控制在125～130℃，乙酸酐和苯酚的摩尔比为0.25∶0.21、反应时间为2.5 h，产率为86％；Fries重排反应的温度应控制在25～30℃，乙酸苯酯和催化剂无水三氯化铝摩尔比为0.15∶0.18、反应时间为24 h，产率为21％；羟醛缩合的反应温度为室温，在稀碱的醇溶液中（0.14 g/mL）进行，反应时间为12 h，产率68％。
以苯酚和乙痠酐為原料，經酚酯化反應、Fries重排反應、羥醛縮閤來閤成4′-羥基查爾酮。對反應的主要因素進行瞭研究，結果錶明：酚酯化反應的溫度應控製在125～130℃，乙痠酐和苯酚的摩爾比為0.25∶0.21、反應時間為2.5 h，產率為86％；Fries重排反應的溫度應控製在25～30℃，乙痠苯酯和催化劑無水三氯化鋁摩爾比為0.15∶0.18、反應時間為24 h，產率為21％；羥醛縮閤的反應溫度為室溫，在稀堿的醇溶液中（0.14 g/mL）進行，反應時間為12 h，產率68％。
이분분화을산항위원료，경분지화반응、Fries중배반응、간철축합래합성4′-간기사이동。대반응적주요인소진행료연구，결과표명：분지화반응적온도응공제재125～130℃，을산항화분분적마이비위0.25∶0.21、반응시간위2.5 h，산솔위86％；Fries중배반응적온도응공제재25～30℃，을산분지화최화제무수삼록화려마이비위0.15∶0.18、반응시간위24 h，산솔위21％；간철축합적반응온도위실온，재희감적순용액중（0.14 g/mL）진행，반응시간위12 h，산솔68％。
4′-Hydroxychalcone was synthesized by acetic anhydride and phenol as raw materials,through es-terification reaction of phenol,Fries rearrangement reaction,and aldol condensation reaction.The influences of main factors on reaction were examined.The results showed that the optimal conditions were the temperatures of esterification 125~130 ℃,the molar ratio of acetic anhydride to phenol 0.25∶0.21 ,the time of the reaction about 2.5 h;the temperatures of Fries rearrangement reaction 25~30 ℃,the molar ratio of phenyl acetate to anhydrous aluminium chloride 0.15∶0.18 ,the time of the reaction about 24 h;the temperatures of aldol con-densation reaction 20~30 ℃,concentration of NaOH 0.14 g/mL,the time of the reaction about 12h.The yield of phenyl acetate can be reached 86%.The yields of 4′-hydroxyacetophone and 4′-Hydroxychalcone can be reached 21 %and 68 %respectively.
