| 9, 9-二(3-氨基-4-羟基苯基)呫吨的合成 |
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| 引用本文： | 方程,姜建文,刘晓玲,盛寿日.9, 9-二(3-氨基-4-羟基苯基)呫吨的合成[J].应用化学,2015,32(1):60-63. |
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| 作者姓名： | 方程 姜建文 刘晓玲 盛寿日 |
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| 作者单位： | 江西师范大学化学化工学院 南昌 330022 |
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| 基金项目： | 国家自然科学基金，江西省自然科学基金，the National Natural Science Foundation of China，the Natural Science Foundation of Jiangxi Province of China |
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| 摘 要： | 以醋酸酐为溶剂, 将9, 9-二(4-羟基苯基)呫吨与浓硝酸在15 ℃左右发生硝化反应1.5 h, 形成中间体-9, 9-二(3-硝基-4-羟基苯基)呫吨, 产率为88.5%;继而以Pd/C 为催化剂, 80%的水合肼为还原剂, 在乙醇和1, 4-二氧六环混合溶剂中, 于70 ℃将中间体进行还原反应10 h, 得到目标产物9, 9-二(3-氨基-4-羟基苯基)呫吨, 产率为90.8%, 两步反应总收率为80.4%。 中间体与目标化合物经NMR、FTIR和元素分析等确定了它们的结构。
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| 关 键 词： | 二(硝基羟基苯基)呫吨 二(氨基羟基苯基)呫吨 硝化反应 还原反应 水合肼 |
| 收稿时间： | 2014-04-14 |
Preparation of 9,9-Bis (3-amino-4-hydroxyphenyl) xanthene |
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| FANG Cheng,JIANG Jianwen,LIU Xiaoling,SHENG Shouri.Preparation of 9,9-Bis (3-amino-4-hydroxyphenyl) xanthene[J].Chinese Journal of Applied Chemistry,2015,32(1):60-63. |
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| Authors: | FANG Cheng JIANG Jianwen LIU Xiaoling SHENG Shouri |
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| Institution: | Institutes of Chemistry and Chemical Engineering, Jiangxi Normal University, Nanchang 330022, China |
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| Abstract: | Treatment of 9, 9-bis(4-hydroxyphenyl)xanthene(1) with nitric acid(69% mass fraction) in acetic anhydride at 15 ℃ for 1.5 h afforded the intermediate, 9, 9-bis(3-nitro-4-hydroxyphenyl)xanthene(2) in 88.5% yield. Compound2was then reduced to the target, 9, 9-bis(3-amino-4-hydroxyphenyl)xanthene(3) in 90.8% yield by hydrazine hydrate in the presence of catalytic amount of Pd/C at 70 ℃ for 10 h in ethanol/dioxane mixed solvents. The two-step overall yield of compound 3 is about 80.4%(based on compound 1). The structures of intermediate2and target compound 3 were characterized by NMR, IR and elemental analysis. |
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| Keywords: | bis (nitro-hydroxyphenyl) xanthene bis (amino-hydroxyphenyl) xanthene nitration reaction |
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