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| 雷尼镍催化加氢合成7-氟-2H-1,4苯并噁嗪-3(4H)-酮 | |
| 引用本文： | 黄引,庞怀林,阳海,黄明智. 雷尼镍催化加氢合成7-氟-2H-1,4苯并噁嗪-3(4H)-酮[J]. 精细化工中间体, 2006, 36(4): 28-29,39 |
| 作者姓名： | 黄引 庞怀林 阳海 黄明智 |
| 作者单位： | 1. 华中师范大学,化学学院,湖北,武汉,430079 2. 湖南师范大学,化学化工学院,湖南,长沙,410081;湖南化工研究院,国家农药创制工程技术研究中心,湖南,长沙,410007 3. 湖南师范大学,化学化工学院,湖南,长沙,410081 4. 湖南化工研究院,国家农药创制工程技术研究中心,湖南,长沙,410007 |
| 基金项目： | 国家“十五”科技攻关项目(2004BA308A23-2)，湖南省科技计划项目(05GK3001) |
| 摘 要： | 研究了雷尼镍为催化剂加氢还原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,使还原、合环一次完成。考察了反应温度、催化剂、氢气压力、时间、溶剂及回收的催化剂和溶剂对反应收率的影响,确定了合成工艺条件:反应温度70℃,反应时间4h,催化剂用量为原料质量的5%,氢气压力5MPa,溶剂甲醇用量为1000mL/mol1。产品的收率92.4%,含量98%,溶剂和催化剂循环使用4次,对收率无影响。产品结构经元素分析、红外光谱、核磁共振确证。 |
| 关 键 词： | 7-氟-2H-1,4苯并噁嗪-3(4H)-酮 雷尼镍 催化加氢 合成 2-(5-氟-2-硝基苯氧基)乙酸甲酯 |
| 文章编号： | 1009-9212（2006）04-0028-02 |
| 收稿时间： | 2006-02-12 |
| 修稿时间： | 2006-02-12 |
Preparation of 7-Fluoro-2H-1,4-benzoxazin-3(4H)-one by Catalytic Hydrogenization |
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| HUANG Yin,PANG Huai-lin,YANG Hai,HUANG Ming-zhi. Preparation of 7-Fluoro-2H-1,4-benzoxazin-3(4H)-one by Catalytic Hydrogenization[J]. Fine Chemical Intermediates, 2006, 36(4): 28-29,39 | |
| Authors: | HUANG Yin PANG Huai-lin YANG Hai HUANG Ming-zhi |
| Affiliation: | 1. Department of Chemistry, Central China Normorl University, Wuhan 430079, China; 2. Department of Chemistry and Chemical Engineering, Hunan Normal University, Changsha 410081, China; 3. National Engineering Research Center for Agrochemicals, Hunan Reseach Institute of Chemical Industry, Changsha 410007, China |
| 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). The yield was 92.4% and the purity was 98%,all the solution and the catalyst could be reclaimed for four times and had no bad effect on the yield and purity. The structure of 2 was comformed by elementary analysis,IR,and 1H NMR. |
| Keywords: | 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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