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3-甲氧基-4-氯-5-硝基苯甲腈(5)是合成美登素的芳香核部分所用的一个中间体.从结构上看,由香兰素(1)来制备5是很值得尝试的.本文报道从1经四步反应制得了5,总产率为11％左右.我们过去由间-二硝基苯经2-甲氧基-6-硝基苯胺等六步反应制得5,总产率仅为7％左右. 1硝化得5-硝基香兰素(2).Grundon曾报道2在甲苯中与磷酰氯及N,N-二乙苯胺共同回流即可得3-甲氧基-4-氯-5-硝基苯甲醛(4).但我们按照其条件重复多次都不能得到所报道的结果,所得产物不是4而是3,即除酚羟基被氯代替外,醛基也已变
3-Methoxy-4-chloro-5-nitrobenzonitrile (5) is an intermediate used in the synthesis of the aromatic nucleus of maytansine.Structurally, 5 from vanillin (1) It is worth to try.This article reports from 1 through four-step reaction was 5, the total yield of about 11% .We used in the past by - 2-nitro-2-nitro-6-nitroaniline and other six-step reaction Obtained in 5, the total yield of only about 7% .1 Nitration of 5-nitro vanillin (2). Grundon has reported 2 in toluene with phosphorus oxychloride and N, N-diethylaniline common reflux can be 3-methoxy-4-chloro-5-nitrobenzaldehyde (4) .But we can not get the reported results by repeated conditions according to its conditions, the resulting product is not 4 but 3, Aldehyde groups have also been changed instead