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尹薰汐: 金币+50, 翻译EPI+1, ★★★★★最佳答案 2016-06-07 15:41:47
本文以 2,4-二氯苯甲醛 和 丙酮 为原料，通过 羟醛缩合 生成4-(2,4-二氯苯基)-3-丁烯-2-酮，再与 过量氨水 合成 药物中间体 7-氯喹哪啶。该 路线 将2,4-二氯苯甲醛 与 过量丙酮 在 氢氧化钠水溶液中 低温搅拌 反应1小时，生成 中间产物 4-(2,4-二氯苯基)-3-丁烯-2-酮。在 催化剂 氧化亚铜的 催化下，以 二甲基甲酰胺 作溶剂 在100 ℃下 反应12小时，得 目标产物 7-氯喹哪啶。通过 调节 原料摩尔比、反应温度 以及 反应时间 等因素，探究 7-氯喹哪啶的 最佳合成条件，收率 可达66.57%。通过 红外光谱、质谱等 表征手段 对产物 进行表征。该路线 安全性高、操作性强，有一定的 工业化前景。
In this paper, based on 2,4-dichlorobenzaldehyde and acetone as raw material, 4-(2,4-dichlorophenyl)-3-butene-2-ketone was first synthesized by method of aldol condensation, and then the drug intermediate-7-Chloro quinaldine was prepared by adding excessive amount of ammonia liquor. By this approach, 2,4-dichlorobenzaldehyde and excessive acetone were subjected to cold mixing in sodium hydroxide solution for 1 h, so that the intermediate product- 4-(2,4-dichlorophenyl)-3-butene-2-ketone can be prepared. Catalyzed by cuprous oxide, reaction was kept at 100 ℃ for 12 h, in which dimethylformamide served as solvent, and thus target product 7-Chloro quinaldine can be obtained. Through adjusting factors such as molar ratio of raw material, reaction temperature, and reaction time, this research explored the optimum synthesis condition of 7-Chloro quinaldine, and found that yield coefficient can reach 66.57%. By characterizing the resulted products using infrared spectroscopy and mass spectrum, it demonstrated that such approach was superior for its higher safety and operability, and of certain prospect of industrialization application. |
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