异烟酸乙酯的相转移催化合成

Synthesis of Ethyl Iso-nicotinate via Phase Transfer Catalysis

以 BTEAC(苄基三乙基氯化铵 )为相转移催化剂合成了异烟酸乙酯。无水乙醇既为溶剂又为反应物 ,所以固定无水乙醇与异烟酸的比例为 1∶ 1 7(摩尔比 ) ,即异烟酸 4.9g( 0 .0 4 mol) ,无水乙醇 40 m L,使无水乙醇大大过量。利用正交实验考察浓 98%H2 SO4(质量分数 ,下同 )用量 ,BTEAC用量 ,反应液最终温度对产率的影响。实验确定了最佳反应条件 :H2 SO45 .5 g,相转移催化剂 0 .3g,最终反应温度 1 0 5°C,收率 82 .6%。在其他条件相同而不加相转移催化剂时收率只有44.6%,实验结果表明相转移催化剂的使用可以提高异烟酸乙酯的产率。

Synthesis of ethyl iso nicotinate using BTEAC (benzyl triethyl ammonium chloride) as phase transfer catalyst was studied. All experiments were performed with the molar ratio of iso nicotinic acid and absolute ethanol equal to 1∶17 since absolute ethanol is used both as the solvent and the reagent. The optimum conditions were: iso nicotinic acid, 4.9 g( 0.04 mol); absolute ethyl alcohol, 40 mL; H 2SO 4 (98%), 5.5 g; BTEAC, 0.3 g; final temperature of reaction, 105 °C . The yield reached 82.6% , and without BTEAC it was reduced to 44.6% .