| 催化加氢合成6-氨基-7-氟-2H-1,4-苯并口恶嗪-3(4H)-酮 |
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| 引用本文： | 阳海,庞怀林,廖文文,黄引,尹笃林,刘智凌.催化加氢合成6-氨基-7-氟-2H-1,4-苯并口恶嗪-3(4H)-酮[J].精细化工,2006(11). |
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| 作者姓名： | 阳海 庞怀林 廖文文 黄引 尹笃林 刘智凌 |
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| 作者单位： | 湖南师范大学化学化工学院，湖南师范大学化学化工学院，湖南师范大学化学化工学院，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 湖南长沙410081，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，湖南长沙410081，湖北武汉430079，湖南长沙410081，湖南长沙410007 |
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| 基金项目： | 国家十五科技攻关项目(No.2004BA308A23-2)，湖南省科技计划项目(No.05GK3001)~~ |
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| 摘 要： | 6-氨基-7-氟-2H-1,4-苯并口恶嗪-3(4H)-酮(Ⅱ)是合成除草剂丙炔氟草胺的关键中间体,该文采用雷尼镍催化加氢还原7-氟-6-硝基-2H-1,4-苯并口恶嗪-3(4H)-酮(Ⅰ)高收率的制得了目标化合物Ⅱ,确定了最佳合成工艺条件:反应温度80℃,反应时间5 h,催化剂用量为原料质量的5%,氢气压力6 MPa,产品的收率95.2%,质量分数98.5%,溶剂和催化剂循环使用5次,对收率和产品质量分数无影响。产品结构经元素分析、红外光谱、核磁共振确证。
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| 关 键 词： | 6-氨基-7-氟-2H-1 4-苯并口恶嗪-3(4H)-酮 雷尼镍 催化加氢 7-氟-6-硝基-2H-1 4-苯并口恶嗪-3(4H)-酮 |
Preparation of 6-Amino-7-fluoro-2H-1,4-benzoxazin-3(4H)-one by Catalytic Hydrogenization |
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| YANG Hai,PANG Huai-lin.Preparation of 6-Amino-7-fluoro-2H-1,4-benzoxazin-3(4H)-one by Catalytic Hydrogenization[J].Fine Chemicals,2006(11). |
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| Authors: | YANG Hai PANG Huai-lin |
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| Affiliation: | YANG Hai~1,PANG Huai-lin~ |
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| Abstract: | 6-Amino-7-fluoro-2H-1,4-benzoxazin-3(4H)-one(Ⅱ),an essential intermediate for synthesis of herbicide flumioxazin,was prepared through hydrogenation of 7-fluoro-6-nitro-2H-1,4-benzoxazin-3(4H)-one(Ⅰ) catalyzed by Raney Ni with high yield.The optimum process conditions were reaction temperature 80 ℃,reaction time 5 h,amount of catalyst 5% based on Ⅰ,and H_2 pressure 6 MPa.The yield was 95.2% and weight percent of Ⅱ was 98.5%.The solvent and the catalyst were reused for five times and showed no bad effect to the yield and weight percent of the product.The structure of Ⅱ was comfirmed by elementary analysis,IR and ~1HNMR. |
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| Keywords: | 6-amino-7-fluoro-2H-1 4-benzoxazin-3(4H)-one Raney Ni catalytic hydrogenation 7-fluoro-6-nitro-2H-1 4-benzoxazin-3(4H)-one |
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