2-吲哚酮和5-甲基-2-吲哚酮的无溶剂法制备

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AICI，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％．

Solvent Free Preparation of 2-Oxindole and 5-Methyl-2-oxindole

N-chloroaeetylanihne was prepared from aniline and chloracetyl chloride in the presence of sodium hydroxide.The resultant product can undergOeyclization-elimination reaction with anhydrous AICl3 as catalyst,giving 2-oxindole.The methodology of synthesizing 2-oxindole was improved.The optimal conditions were as follows:the reaction temperature 220℃,the reaction time 60 min,the charging-up temperature 180℃ and the mass ratiOof N-chloroacetylanihne/sodium chloride/anhy-drous aluminium chloride 1:1:5.5.The yield was 88.3%.24.6%higher than literature with 99% purity.Based on this method,5-methyl-2-oxindole was synthesized and the optimal conditions were as follows:the reaction temperature 190℃,the reaction time 30 min,the charging-up temperature 180 ℃ and the mass ratiOof 2-choro-N-p-tolyl-acetamide/sodium chloride/anhydrous aluminium chloride 1:1:5.5.The yield was 83.1% with purity of 99%.