7-甲氧基-4-(2-甲基-4-喹唑啉基)-3,4-二氢喹噁啉-2(1H)-酮的合成工艺改进
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篇名: 7-甲氧基-4-(2-甲基-4-喹唑啉基)-3,4-二氢喹噁啉-2(1H)-酮的合成工艺改进
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摘要: 目的:改进7-甲氧基-4-(2-甲基-4-喹唑啉基)-3,4-二氢喹噁啉-2(1H)-酮的合成工艺。方法:以2-甲基-4(3H)-喹唑啉酮为起始原料,通过氯代、亲核取代、二芳胺烷基化和硝基还原环合等反应对7-甲氧基-4-(2-甲基-4-喹唑啉基)-3,4-二氢喹噁啉-2(1H)-酮的合成工艺进行改进,并考察其收率。结果:7-甲氧基-4-(2-甲基-4-喹唑啉基)-3,4-二氢喹噁啉-2(1H)-酮的结构经核磁共振氢谱和电喷雾质谱确证,总收率为43.5%,较改进前的20.2%提高了23.3%。结论:改进后的工艺更简单,条件更温和,适合实验室研究的批量制备。
ABSTRACT: OBJECTIVE:To improve the synthesis technology of 7-methoxy-4-(2-methyl-4-quinazolinyl)-3,4-dihydroquinoxalin-2(1H)-ketone. METHODS: Using 2-methyl-4(3H)-quinazolone as starting material, the synthesis technology of 7-methoxy-4-(2-methyl-4-quinazolinyl)-3,4-dihydroquinoxalin-2(1H)-ketone was improved by clorination, nucleophilic substitution, diarylamine alkylation and nitro reductive cyclization. The yield of it was investigated. RESULTS: The structure of 7-methoxy-4-(2-methyl-4-quinazolinyl)-3,4-dihydroquinoxalin-2(1H)-ketone had been verified by 1H-NMR and ESI-MS. The yield was 43.5% and improved by 23.3% compared to 20.2% before improvement. CONCLUSIONS: Improved technology is simpler and milder, which is suitable for the batch preparation of laboratory study.
期刊: 2018年第29卷第6期
作者: 史疆,地里夏提·白克力,张晨,鄂晓,尹东锋,王晓锋
AUTHORS: SHI Jiang,DILIXIATI·Baikeli,ZHANG Chen,E Xiao,YIN Dongfeng,WANG Xiaofeng
关键字: 7-甲氧基-4-(2-甲基-4-喹唑啉基)-3,4-二氢喹噁啉-2(1H)-酮;合成工艺;2-甲基-4(3H)-喹唑啉酮;改进
KEYWORDS: 7-methoxy-4-(2-methyl-4-quinazolinyl)-3,4-dihydroquinoxalin-2(1H)-ketone; Synthesis technology; 2-methyl-4(3H)-quinazolone; Improvement
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