| 2-甲氧基-4'-三氟甲基苯乙酮的合成 |
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| 引用本文： | 宋秀娟,覃志忠,张国亮,张凤宝,戈建华.2-甲氧基-4'-三氟甲基苯乙酮的合成[J].高校化学工程学报,2005,19(3):414-417. |
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| 作者姓名： | 宋秀娟 覃志忠 张国亮 张凤宝 戈建华 |
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| 作者单位： | 天津大学,化工学院,天津,300072;沧州华光化工有限公司,河北,沧州,061600 |
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| 摘 要： | 以4-三氟甲基苯甲酸甲酯和甲氧基乙酸甲酯为原料，在碱性条件下进行交叉酯缩合反应，然后经水解、脱羧得到产品2-甲氧基-4′-三氟甲基苯乙酮，总收率达85％以上。实验获得了较佳工艺条件：原料配比4-三氟甲基苯甲酸甲酯／甲氧基乙酸甲酯为1／1．5(mol／mol)，酯缩合的反应温度为30℃、反应时间为12h，适宜的溶剂为DMSO：水解、脱羧反应时间为15h；并采用^1HNMR及IR对产品进行了表征。
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| 关 键 词： | 2-甲氧基-4’-三氟甲基苯乙酮 4-三氟甲基苯甲酸甲酯 甲氧基乙酸甲酯 交叉酯缩合 水解 脱羧 |
| 文章编号： | 1003-9015(2005)03-0414-04 |
| 修稿时间： | 2004年1月19日 |
Synthesis of 2-Methoxy-4'-trifluoromethyl Acetophenone |
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| SONG Xiu-juan,QIN Zhi-zhong,ZHANG Guo-liang,ZHANG Feng-bao,GE Jian-hua.Synthesis of 2-Methoxy-4'-trifluoromethyl Acetophenone[J].Journal of Chemical Engineering of Chinese Universities,2005,19(3):414-417. |
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| Authors: | SONG Xiu-juan QIN Zhi-zhong ZHANG Guo-liang ZHANG Feng-bao GE Jian-hua |
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| Affiliation: | SONG Xiu-juan1,QIN Zhi-zhong2,ZHANG Guo-liang1,ZHANG Feng-bao1,GE Jian-hua2 |
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| Abstract: | A new method was proposed to prepare 2-methoxy-4'-trifluoromethyl acetophenone with higher yield and simpler operation conditions. Starting from methyl 4-trifluoromethyl benzoate (TFMB) and methyl methoxyacetate (MTA), the title compound was prepared via cross ester condensation, hydrolysis and decarboxylation with overall yield higher than 85%. The effects of reaction time, temperature, feeds molar ratio and solvent on the conversion of ester condensation were investigated, and the optimum reaction conditions were obtained as following: TFMB / MTA 1/1.5 (molar ratio), the cross ester condensation time 12h, the hydrolysis and decarboxylation time 15h; the cross ester condensation temperature 30?C, and the suitable solvent for this condensation reaction is dimethyl sulfoxide (DMSO). |
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| Keywords: | 2-methoxy-4'-trifluoromethyl acetophenone methyl 4-thrifluoromethyl benzoate methyl methoxyacetate cross ester condensation hydrolysis decarboxylation |
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