腐殖酸催化醛高效快速合成腈

Efficient and Rapid Synthesis of Nitriles from Aldehydes Catalyzed by Humic Acid

腐殖酸是一种无毒、非金属、价格低廉和来源广泛的大分子有机物质。以腐殖酸为催化剂,N-甲基吡咯烷酮(NMP)为溶剂,由醛和盐酸羟胺反应合成了腈类化合物。研究了催化剂用量、溶剂、反应温度等因素对产率的影响。实验结果表明:醛1.0 mmol,盐酸羟胺1.2 mmol,催化剂腐殖酸0.1 g,NMP 2 mL,在110℃下反应5~8 min可以获得较高产率的产物。所有化合物的结构经^(1)H NMR和^(13)C NMR确证。该法具有产物收率高、操作简便、反应时间短、催化剂绿色并可重复使用等优点。

Humic acid is a non-toxic,non-metallic,inexpensive and widely available high-molecular weight polymer.A simple and efficient approach for the synthesis of nitriles from aldehydes and hydroxylamine hydrochloride using humic acid as the catalyst in N-methyl pyrrolidone(NMP)had been developed.The effects of catalyst dosage,solvent and reaction temperature on the reaction were discussed.The results showed that the optimum conditions were as followed:1.0 mmol of aldehydes,1.2 mmol of hydroxylamine hydrochloride,0.1 g of catalyst humic acid,2 mL of NMP,reaction temperature 110℃,reaction time 5~8 min.The structures of target compounds were characterized by ^(1)H NMR and ^(13)C NMR.The method reported has several advantages such as high to excellent yields,easy work-up,short reaction time,use of green and reusable catalyst.