| 第 36 卷第 4 期 |  | Vol. 36 No. 4 | | 2006 年 8 月 | Aug 2006 |
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所屬欄目：農藥及中間體
雷尼鎳催化加氫合成7-氟-2H-1,4苯并噁嗪-3(4H)-酮 |
| 黃引; 龐懷林; 陽(yáng)海; 黃明智(華中師范大學(xué)化學(xué)學(xué)院; 湖南師范大學(xué)化學(xué)化工學(xué)院; 湖南化工研究院國家農藥創(chuàng )制工程技術(shù)研究中心; 湖北武漢; 湖南長(cháng)沙410081湖南化工研究院國家農藥創(chuàng )制工程技術(shù)研究中心; 湖南長(cháng)沙) |
| 摘 要：研究了雷尼鎳為催化劑加氫還原2-(5-氟-2-硝基苯氧基)乙酸甲酯(1)合成7-氟-2H-[1,4]苯并噁嗪-3(4H)-酮(2)的方法,使還原、合環(huán)一次完成�？疾炝朔磻獪囟�、催化劑、氫氣壓力、時(shí)間、溶劑及回收的催化劑和溶劑對反應收率的影響,確定了合成工藝條件:反應溫度70℃,反應時(shí)間4h,催化劑用量為原料質(zhì)量的5%,氫氣壓力5MPa,溶劑甲醇用量為1000mL/mol1。產(chǎn)品的收率92.4%,含量98%,溶劑和催化劑循環(huán)使用4次,對收率無(wú)影響。產(chǎn)品結構經(jīng)元素分析、紅外光譜、核磁共振確證。 |
| 關(guān)鍵詞：7-氟-2H-1; 4苯并噁嗪-3（4H）-酮; 雷尼鎳; 催化加氫; 合成; 2-（5-氟-2-硝基苯氧基）乙酸甲酯 |
| 中圖分類(lèi)號：TQ244.4 文獻標識碼：A 文章編號：1009-9212(2006)04-0028-02 |
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| Preparation of 7-Fluoro-2H-1,4-benzoxazin-3(4H)-one by Catalytic Hydrogenization |
| HUANG Yin;PANG Huai-lin;YANG Hai;HUANG Ming-zhi(Department of Chemistry;Central China Normorl University;Department of Chemistry and Chemical Engineering;Hunan Normal University;National Engineering Research Center for Agrochemicals....) |
| Abstract：7-Fluoro-2H-1,4-benzoxazin-3(4H)-one(2) was prepared through the reaction of hydrogenization catalyzed by Rany Nickel from methyl 2-(5-fluoro-2-nitrophenoxy) acetate(1). The effect of temperature,catalyst,pressure of H2,reaction time,solvents and reclaim of all the solution and the catalyst were investigated. The optimum process conditions were determined as following:Reaction temperature was 70℃,time 4 h,the catalyst amount 5% comparing to 1 (w/w),the hydrogen pressure 5 MPa and methanol 1 000 mL/mol(1). T... |
| Key words：7-fluoro-2H-1; 4-benzoxazin-3（4H）-one; Rany Ni; catalytic hydrogenization; preparation; methyl 2-（5-fluoro-2-nitrophenoxy）acetate |
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基金項目：國家“十五”科技攻關(guān)項目(2004BA308A23-2);湖南省科技計劃項目(05GK3001)
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收稿日期：2006-02-12
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