摘要
2-噻吩甲酸(T2)是杀线虫剂Tioxazafen的关键中间体。以噻吩和乙酰氯为原料制备2-噻吩乙酮(T1),随后用次氯酸钠氧化得到产品2-噻吩甲酸(T2)。T1的优化制备条件为:n(噻吩)∶n(乙酰氯)∶n(三氯化铝)=1.00∶1.15∶1.15,反应温度为25℃,噻吩滴加到乙酰氯和三氯化铝的二氯乙烷溶液中;T2的优化制备条件为:n(T1)∶n(次氯酸钠)=1.00∶3.15,氧化温度为30℃。2步反应总收率87.84%,纯度98.23%(HPLC)。
2-Thiophenecarboxylic acid(T2)is a key intermediate of the nematicideTioxazafen.2-Thiophene ethyl ketone(T1)was prepared fromthiophene and acetyl chloride.And then T1 was oxidized using sodium hypochlorite to give the product T2.The optimized preparation conditions of T1 were as followings:a molar ratiobewteenthiophene,acetyl chloride and aluminum trichloride was of 1.00∶1.15∶1.15;the reaction temperature was of 25℃;thiophene was added dropwise to a solution of acetyl chloride and aluminum trichloride in dichloroethane.The optimized preparation conditions of T2 were as followings:the oxidation temperature was of 30℃;and n(T1)∶n(sodium hypochlorite)was of 1.00∶3.15.The total yield of the two-step reactions was 87.84%with a purity of 98.23%(HPLC).
作者
张广平
王梓鉴
ZHANG Guang-ping;WANG Zi-jian(Hunan Haili Changde Pesticide Chemical Co.,Ltd.,Changde 415001,China;Chang Sha Jia Qiao Biotech Co.,Ltd.,Changsha 410000,China)
出处
《精细化工中间体》
CAS
2020年第4期18-20,68,共4页
Fine Chemical Intermediates
基金
国家自然科学基金项目(21672057)。
