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丙腈合成2-乙基-4,6-二羟基嘧啶的研究

Synthesis of 2-ethyl-4, 6-dihydroxypyrimidine

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【作者】 欧春艳张竞陈声宗吴宏宋来峰

【Author】 OU Chun-yan, ZHANG Jing, CHEN Sheng-zong, WU Hong ,SONG Lai-feng (College of Science,Zhanjiang Ocean University,Zhanjiang 524088;College of Chemistry & Chemical Engineering, Hunan University, Chang-sha,410082)Huaxue Shiji,2003,25(5),296 - 298

【机构】 湛江海洋大学理学院湖南大学化学化工学院湖南大学化学化工学院 广东湛江524088湖南长沙410082湖南长沙410082

【摘要】 以丙腈为原料,与氯化氢、氨气反应合成丙脒盐酸盐,然后在醇钠催化下与丙二酸二乙酯缩合成环制得2-乙基-4,6-二羟基嘧啶,反应总收率为86%,产品分别经熔点测定、质谱分析得到了证实,含量经液相色谱分析,纯度均大于98%。另外,在合成丙脒盐酸盐时,必须在无水条件下进行,而且在通入氯化氢气体时,反应温度保持在-10~0℃,其反应收率为94.0%。

【Abstract】 2-Ethyl-4, 6-dihydroxypyrimidine was synthesized , with propionitrile as starting material, by reacting with hydrogen chloride and free ammonia, then in the presence of sodium methoxide by means of cyclization of diethyl malonuric esters with propionamide hydrochloride in 86% yield. The structures of these compounds were confirmed by MS and melting point. Their purity was better than 98%, analyzed by LC. The optimum conditions for synthesizing propionamide hydrochloride were exclusion of moisture and keeping the reaction temperature at -10 - 0℃, when hydrogen chloride gas was led in, its yield was 94. 0%.

【基金】 国家重点攻关项目(2002BA328C)
  • 【分类号】O626
  • 【被引频次】8
  • 【下载频次】317
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