5-1-(甲硫基)乙基-2-(三氟甲基)吡啶的合成工艺研究

Study on the Synthesis of 5-(1-methylthio)ethyl-2-(trifluoromethyl)pyridine

以3-(3-甲硫基丁-1-烯基)吡咯烷(1)为原料,在氮气保护和碳酸氢铵存在下与4-乙氧基-1,1,1-三氟丁-3-烯-2-酮(2)反应,合成化合物5-1-(甲硫基)乙基-2-(三氟甲基)吡啶(3)。反应收率达到63.5%,产品含量为98.6%。考察了反应条件对反应收率的影响,确定了优惠的合成工艺条件:物料配比n(1)∶n(2)∶n(碳酸氢铵)=0.9∶1.0∶2.2,反应溶剂为乙腈,溶剂用量为250mL/mol(以化合物2计),反应的保温温度为75℃,反应总时间为4.5h。

5-（1-methyhhio）ethyl-2-（trifluoromethyl）pyridine（_3）was synthesized from 1-（3-methylthiobut-1- phenyl） pyrrolidine （1） and 4-ethoxy- 1, l, 1-trifluoro-but-3-en-2-one （2）in the protection of nitrogen and presence of ammonium formate. The yield of the reaction was about 63.5% with the purity of 98.6%. The effect of the reaction conditions on reaction yield was investigated, and the optimal conditions were as follows： the material ratio of n （ 1 - （ 3-methyhhiobut- 1 -phenyl ） pyrrolidine ）： n （ 4-ethoxy- 1,1,1 -trifluoro-but-3-en-2-one ）： n（ammonium biearbonate）=0.9：1.0：2.2, reaction solvent was acetonitrile, the solvent amount was 250 mL/mol, ealefactive reaction temperature was 75 ℃, total reaction time was 4.5 hours.