合成2-(3-噻吩基)丙二酸的新工艺

设计了合成2-(3-噻吩基)丙二酸的新路线,采用配位催化碘化法,以3-溴噻吩为原料,经碘代、缩合和水解、酸化等反应合成2-(3-噻吩基)丙二酸。在正丁醇中,3-溴噻吩在CuI/N,N′-二甲基乙二胺催化下与KI进行碘代反应,得到3-碘噻吩,收率为91.73%;3-碘噻吩再在CuBr催化下与丙二酸二乙酯钠盐进行缩合反应,制得2-(3-噻吩基)丙二酸二乙酯,收率为76.30%;2-(3-噻吩基)丙二酸二乙酯经水解和酸化反应后得到最终产品2-(3-噻吩基)丙二酸,收率为82.63%。该路线合成2-(3-噻吩基)丙二酸的总收率(以3-溴噻吩计)为57.83%。

New Synthesis Process for 2-(3-Thienyl) Malonic Acid

2-(3-Thieny1) malonic acid was synthesized from 3-bromothiophene with coordinative catalyst,through a new route,namely iodination,condensation,hydrolysis and acidification.3-Bromothiophene reacted with KI in n-butanol with CuI/N,N'-dimethylethane-1,2-diamine as catalyst system.Yield of obtained 3-iodothiophene reaches 91.73%.The 3-iodothiophene converted to diethyl 2-(3-thieny1)malonate by condensation with sodium salt of diethyl malonate in presence of CuBr as catalyst.Yield of obtained diethyl 2-(3-thieny...