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以苯甲醛与异Vc为原料,N,N-二甲基乙酰胺为溶剂,甲基磺酸为催化剂,环己烷为带水剂,合成了苯甲醛异Vc缩醛。用正交实验法考察了原料配比、催化剂用量、溶剂用量和回流温度对反应收率的影响,最佳条件为:苯甲醛、异Vc与甲基磺酸的物质的量的比为1mol∶1.5mol∶0.25mol、溶剂用量0.75L、回流温度120℃、反应时间4.0h,收率可达73.9%。产物结构用IR、MS和元素分析确认。
Benzaldehyde and iso Vc as raw materials, N, N-dimethylacetamide as solvent, methanesulfonic acid as catalyst, and cyclohexane as water-bearing agent. The effects of the ratio of raw materials, the amount of catalyst, the amount of solvent and the reflux temperature on the yield of the reaction were investigated by orthogonal experiment. The optimum conditions were as follows: the ratio of the amount of benzaldehyde, iso Vc and methanesulfonic acid was 1mol: 1.5mol: 0.25mol, the amount of solvent 0.75L, reflux temperature 120 ℃, reaction time 4.0h, yield up to 73.9%. The product structure was confirmed by IR, MS and elemental analysis.