第 36 卷第 4 期 Vol. 36 No. 4 2006 年 8 月 Aug 2006

所属栏目：农药及中间体 雷尼镍催化加氢合成7-氟-2H-1,4苯并噁嗪-3(4H)-酮

黄引; 庞怀林; 阳海; 黄明智(华中师范大学化学学院; 湖南师范大学化学化工学院; 湖南化工研究院国家农药创制工程技术研究中心; 湖北武汉; 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)

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

中图分类号：TQ244.4　　文献标识码：A　　文章编号：1009-9212(2006)04-0028-02

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

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)

收稿日期：2006-02-12

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