| 6,11-二氢二苯骈[b,e]氧杂-11-酮-2-乙酸的合成 |
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| 引用本文： | 汪淼,杨艺虹,张珩,杨建设,吴春姗. 6,11-二氢二苯骈[b,e]氧杂-11-酮-2-乙酸的合成[J]. 精细化工中间体, 2007, 0(2) |
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| 作者姓名： | 汪淼 杨艺虹 张珩 杨建设 吴春姗 |
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| 作者单位： | 武汉工程大学湖北省新型反应器与绿色化学工艺重点实验室 湖北武汉430073 |
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| 摘 要： | 采用对羟基苯乙酸(Ⅱ)和苯酞为原料,在甲醇钠的催化下,以n(Ⅱ)∶n(苯酞)∶n(甲醇钠)=1.0∶1.1∶2.2,于130℃反应7h制备4-(2-羧基苄氧基)苯乙酸(Ⅲ)。Ⅲ与乙酰氯经氯化、环合得6,11-二氢二苯骈[b,e]氧杂-11-酮-2-乙酸(Ⅰ),该步优化的反应条件为:n(Ⅲ)∶n(乙酰氯)=1∶1.25,反应温度为100℃,反应时间为6h。以Ⅱ计,总收率达48.16%,Ⅰ的结构经IR、1H NMR和MS确证。
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| 关 键 词： | 对羟基苯乙酸 苯酞 4-(2-羧基苄氧基)苯乙酸 环合 |
Synthesis of 6,11-Dihydro-11-oxodibenz[b,e]oxepin-2-acetic Acid |
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| WANG Miao,YANG Yi-hong,ZHANG Heng,YANG Jian-she,WU Chun-shan. Synthesis of 6,11-Dihydro-11-oxodibenz[b,e]oxepin-2-acetic Acid[J]. Fine Chemical Intermediates, 2007, 0(2) |
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| Authors: | WANG Miao YANG Yi-hong ZHANG Heng YANG Jian-she WU Chun-shan |
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| Abstract: | 4-(2-Carboxybenzyloxy)phenylacetic acid (Ⅲ)was synthesized from 4-Hydroxyphenyl acetic acid(Ⅱ)and phthalide in the presence of the catalyst sodium methoxide. The molar ratio of reactants(Ⅱ ∶ phthalide ∶ sodium methoxide)was 1.0 ∶ 1.1 ∶ 2.2,the reaction time was 7 h and reaction temperature was 130℃. 6,11-Dihydro-11-oxodibenz[b,e]oxepin-2-acetic acid(Ⅰ) was synthesized from Ⅲand acetyl chloride through two-step reactions including chlorination and cyclization. The optimum reaction conditions were as follows:n(Ⅲ) ∶ n(acetyl chloride)=1 ∶ 1.25,reaction time 6 h and reaction temperature 100℃. The overall yield that was calculated from Ⅱ was 48.16%. Structure of Ⅰ was characterized by IR,1H NMR and MS. |
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| Keywords: | 4-hydroxyphenyl acetic acid phthalide 4-(2-carboxybenzyloxy)phenylacetic acid cyclization |
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