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9,9-二(3-氨基-4-羟基苯基)呫吨的合成与表征
引用本文:胡美琴,魏梅红,李翛,邓伟,盛寿日.9,9-二(3-氨基-4-羟基苯基)呫吨的合成与表征[J].江西师范大学学报(自然科学版),2014,0(4):342-345.
作者姓名:胡美琴  魏梅红  李翛  邓伟  盛寿日
作者单位:江西师范大学化学化工学院,江西 南昌,330022
基金项目:国家自然科学基金,江西省主要学科学术和技术带头人培养计划,江西省自然科学基金
摘    要:将9,9-二(4-羟基苯基)呫吨与质量浓度为20;的稀硝酸在10~15℃下发生硝化反应约3 h,以86.5;的产率合成了中间体9,9-二(3-硝基-4-羟基苯基)呫吨,然后以10;的 Pd/ C 和甲醇为催化剂/溶剂体系,采用加氢还原方法,在75~80℃将中间体还原得到9,9-二(3-氨基-4-羟基苯基)呫吨,产率为92.7;,2步反应总收率为80.2;,并用1 H NMR、IR 和元素分析等方法证实了上述2种化合物的结构.

关 键 词:9  9-二(4-羟基苯基)呫吨  9  9-二(3-硝基-4-羟基苯基)呫吨  9  9-二(3-氨基-4-羟基苯基)呫吨

The Synthesis and Characterization of 9,9-Bis(3-Anino-4-HydroxyPhenyl)Xanthene
HU Mei-qin,WEI Mei-hong,LI Xiao,DENG Wei,SHENG Shou-ri.The Synthesis and Characterization of 9,9-Bis(3-Anino-4-HydroxyPhenyl)Xanthene[J].Journal of Jiangxi Normal University (Natural Sciences Edition),2014,0(4):342-345.
Authors:HU Mei-qin  WEI Mei-hong  LI Xiao  DENG Wei  SHENG Shou-ri
Institution:HU Mei-qin;WEI Mei-hong;LI Xiao;DENG Wei;SHENG Shou-ri;College of Chemistry and Chemical Engineering,Jiangxi Normal University;
Abstract:Nitration between 9,9-bis(4-hydroxyphenyl)xanthene(1)with 20; aqueous HNO3 15 ~ 20 ℃ for 3 h yielded 9,9-bis(3-nitro-4-hydroxyphenyl)xanthene(2)in 86. 5; yield,which was further converted to 9,9-bis(3-amino-4-hydroxyphenyl)xanthene(3)in 92. 7; yield by reduction with hydrogen in the presence of catalytic amount of Pd / C at 75 ~ 80 ℃ for 1 h in methanol solvent. The two-step overall yield of 3 was about 80. 2;(based on compound 1)and their structures of 2 and 3 were characterized by 1 H NMR,IR and elemental analysis tech-nique.
Keywords:9  9-bis(4-hydroxyphenyl)xanthene  9  9-bis(3-nitro-4-hydroxyphenyl)xanthene  9  9-bis(3-amino-4-hydroxyphenyl)xanthene  nitration reaction  catalytic hydrogenation  reduction reaction  synthesis and characteriza-tion
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