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以苯胺和氯乙酰氯为原料在NaOH存在下酰化合成N-氯乙酰基苯胺,然后N-氯乙酰基苯胺在无水AlCl3催化下环化合成2-吲哚酮.对由N-氯乙酰基苯胺合成2-吲哚酮的工艺条件进行了改进.结果表明合成2-吲哚酮的最佳条件为:反应温度为220℃,反应时间为60min,加料时温度为180℃,N-氯乙酰基苯胺与氯化钠,无水AlCl3的重量比为1∶1∶5.5.改进后的合成2-吲哚酮收率达到88.3%,纯度99%,收率比原工艺提高了24.6%.在此基础上,还合成了5-甲基-2-吲哚酮,并得到其最佳条件为:反应温度为190℃,反应时间为30min,加料时温度为180℃,4-甲基-N-氯乙酰基苯胺与氯化钠,无水AlCl3的重量比为1∶1∶5.5,收率达到83.1%,纯度为99%.
Aniline and chloroacetyl chloride are used as raw materials to acylate N-chloroacetyl aniline in the presence of NaOH and then N-chloroacetylanilide is cyclized to synthesize 2-indolone under anhydrous AlCl3 catalysis. The results showed that the optimum conditions for the synthesis of 2-indolone were as follows: the reaction temperature was 220 ℃, the reaction time was 60 min, the temperature was 180 ℃ when adding aniline, N-chloro The weight ratio of acetylaniline to sodium chloride and anhydrous AlCl3 is 1: 1: 5.5.The improved yield of 2-indolone reached 88.3% with a purity of 99% and the yield was 24.6% higher than that of the original one. On this basis, 5-methyl-2-indolone was also synthesized and the optimum conditions were as follows: the reaction temperature was 190 ℃, the reaction time was 30min, the temperature was 180 ℃, N-chloroacetylaniline and sodium chloride, anhydrous AlCl3 weight ratio of 1: 1: 5.5, the yield was 83.1%, a purity of 99%.