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1H-3-正丙基-5-吡唑羧酸乙酯的合成 被引量:1

SYNTHESIS OF 1H-3-n-PROPYL PYRAZOLE-5-CARBOXYLIC ACID ETHYL ESTER
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摘要 2-戊酮和草酸二乙酯在醇钠溶液中发生 Claisen酯缩合反应 ,制得的δ-庚酮酸乙酯 -β-烯醇钠盐收率为 69.2 % ,该钠盐与水合肼及硫酸肼反应制得 1 H- 3-正丙基 - 5 -吡唑羧酸乙酯 ,粗产品收率为 1 0 0 % .通过正交实验及单因素实验研究了反应的较佳合成工艺条件 ,用红外光谱对产品进行了结构鉴定 . The Claisen condensation of 2 pentanone with diethyloxalate yielded sodium 1 ethoxycarbonyl 3 oxo hexanolate. Treatment of this sodium compound with the mixture of hydrazine hydrate and hydrazine sulfate solution gave 1H 3 n propyl pyrazole 5 carboxylic acid ethyl ester. The effective conditions of each step were acquired through orthogonal test or single factor test,and the reaction mechanism was also studied. The structures of the products were identified by analysis of IR spectrometry.
出处 《北京工商大学学报(自然科学版)》 CAS 2002年第4期11-13,35,共4页 Journal of Beijing Technology and Business University:Natural Science Edition
关键词 合成 2-戊酮 δ-庚酮酸乙酯-β-烯醇钠盐 1H-3-正丙基-5-吡唑羧酸乙酯 Claisen酯缩合反应 医药中间体 pentanone Sodium 1 ethoxycarbonyl 3 oxo hexanolate 1H 3 n propyl pyrazole 5 carboxylic acid ethyl ester
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  • 1Yamanaka H. Synthesis of heteroaromatic carboxylic acids closely related to fusaric acid[J]. Chem Pharm Bull, 1983,31(12):4549-4553.
  • 2Rubessa R. Synthesis of pyrazole derivatives[J]. Farmaco Ed Sci,1967,22(9):692-697.
  • 3Posner G H. One-flask consecutive[3,3]and [2,3]sigmatropic rearrangements for conversions of propargylic alcohols into two-carbon-extended 4-Oxo-2-alkenoate esters[J]. J Org Chem, 1991,56:6897-6913.
  • 4Seki K. Studies on hypolipidemic agents Ⅱ synthesis and pharmacological properties of alkylpyrazole derivatives[J]. Chem Pharm Bull, 1984,32(4):1568-1577.

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