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本文用3,4,5-三甲氧基苯甲酰氯(Ⅰ),先生成1-酰基-2-氰基-1,2-二氢喹啉衍生物,再以硫酸水解而得3,4,5-三甲氧基苯甲醛(TMBA)。即在0.16MNaCN的水溶液中,加入0.17M喹啉的二氯甲烷溶液再滴加0.167MⅠ的二氯甲烷溶液,搅拌反应,得1,2-二氢-1-(3,4,5-三甲氧基苯甲酰)-2-喹啉羧基腈(Ⅱ),收率95％。0.03MⅡ,加30％硫酸 400ml,快速搅拌,107℃回流反应,至成均相的橙色溶液,提取所得粗品用沸环己烷溶解,过滤,得0.5g不溶物,为Ⅱ,滤液冷却得白色TMBA,收率95％。融点75～77℃。上述
In this paper, 3,4,5-trimethoxybenzoyl chloride (Ⅰ), the precursor into 1-acyl-2-cyano-1,2-dihydroquinoline derivatives, and then sulfuric acid hydrolysis 3,4, 5-Trimethoxybenzaldehyde (TMBA). That is 0.16MNaCN aqueous solution was added 0.17M quinoline in methylene chloride solution was added dropwise 0.167MⅠ methylene chloride solution and stirred to give 1,2-dihydro-1- (3,4,5-trimethyl Oxybenzoyl) -2-quinolinecarboxycarbonitrile (II) in 95% yield. 0.03M ¢ ò, add 30% sulfuric acid 400ml, stir rapidly and reflux at 107 ° C to a homogeneous orange solution. The crude product was extracted with boiling cyclohexane and filtered to give 0.5g of insoluble material, II, the filtrate was cooled to white TMBA, yield 95%. Melting point 75 ~ 77 ℃. Above