【作者】 刘安昌； 汪鲁焱； 郑怡倩；

【Author】 LIU An-chang;ZHEN Yi-qian;WANG Lu-yan;Wuhan Institute of Technology Chemistry and Environment School;

【机构】 武汉工程大学化学与制药学院；

【摘要】 以2-氯-5-氯甲基吡啶为起始原料,在三乙胺的作用下与2,2-二氟乙胺反应得到N-((6-氯-3-吡啶)甲基)-2,2-二氟乙胺;以丙二酸二甲酯为原料,与氢氧化钾反应,得到丙二酸甲酯单钾盐,然后在相转移催化剂四丁基溴化胺的作用下,与氯乙酸甲酯反应生成2-甲氧基-2-氧代乙基丙二酸甲酯,随后进行分子内关环得到4-羟基-2-氧-2,5-二氢-3-呋喃甲酸甲酯钠盐。最后N-((6-氯-3-吡啶)甲基)-2,2-二氟乙胺与4-羟基-2-氧-2,5-二氢-3-呋喃甲酸甲酯钠盐反应得到目的产物氟吡呋喃酮,总收率50.8%(以丙二酸二甲酯计算)。更多还原

【Abstract】 In the present of triethylamine,N-[(6-chlorpyridin-3-yl)methyl)-2,2 difluorethylamin was prepared by the reaction of 2-chloro-5-chloromethylpyridine with 2,2-difluoroethylamine;Malonic acid dimethyl reacted with potassium hydroxide to give the methyl malonate monopotassium salt,then in the present of the phase transfer catalyst tetrabutylammonium bromide,the methyl malonate monopotassium salt reacted with methyl chloroacetate to the methy 2-methoxy-2-oxoethylpropanedicarboxylate;Then it was closed cycle by intramolecula to gave sodium 4-(ethoxycarbonyl)-5-oxo-2,5-dihydrofuran-3-oxid;At last,the sodium4-(ethoxycarbonyl)-5-oxo-2,5-dihydrofuran-3-oxid reacted with N-[(6-chlorpyridin-3-yl)methyl)-2,2 difluorethylamin to give the target production of flupyradifurone,the total yield was above50.8%.(Calculated by dimethyl malonate)更多还原