[1]胡美琴,魏梅红,李翛,等.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,(04):342-345.
 HU Mei-qin,WEI Mei-hong,LI Xiao,et al.The Synthesis and Characterization of 9,9-Bis(3-Anino-4-HydroxyPhenyl)Xanthene[J].Journal of Jiangxi Normal University:Natural Science Edition,2014,(04):342-345.
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9,9-二(3-氨基-4-羟基苯基)呫吨的合成与表征()
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《江西师范大学学报》(自然科学版)[ISSN:1006-6977/CN:61-1281/TN]

卷:
期数:
2014年04期
页码:
342-345
栏目:
出版日期:
2014-08-31

文章信息/Info

Title:
The Synthesis and Characterization of 9,9-Bis(3-Anino-4-HydroxyPhenyl)Xanthene
作者:
胡美琴;魏梅红;李翛;邓伟;盛寿日
江西师范大学化学化工学院,江西 南昌,330022
Author(s):
HU Mei-qin;WEI Mei-hong;LI Xiao;DENG Wei;SHENG Shou-ri
关键词:
99-二(4-羟基苯基)呫吨99-二(3-硝基-4-羟基苯基)呫吨99-二(3-氨基-4-羟基苯基)呫吨
Keywords:
99-bis(4-hydroxyphenyl)xanthene99-bis(3-nitro-4-hydroxyphenyl)xanthene99-bis(3-amino-4-hydroxyphenyl)xanthenenitration reactioncatalytic hydrogenationreduction reactionsynthesis and characteriza-tion
分类号:
O625
文献标志码:
A
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.
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.

参考文献/References:

[1] Wolfe J F,Arnold F E.Rigid-rod polymers.1.Synthesis and thermal properties of para-aromatic polymers with 2,6-benzobisoxazole units in the main chain [J].Macromolecules,1981,14(4):909-915.
[2] 袁江,王建营,胡文祥,等.聚苯并噁唑(PBO)的合成及其应用研究 [J].化工时刊,2003,17(8):4-8.
[3] 费斐,虞鑫海.聚苯并噁唑树脂的合成及其应用 [J].绝缘材料,2008,41(6):8-13.
[4] Hsiao S H,He M H.Synthesis and properties of novel cardo aromatic poly(ether-benzoxazole)s [J].J Polym Sci,Part A:Polym Chem,2001,39(22):4014-4021.
[5] Huang Wei,Li Shujing,Du Chunping,et al.Synthesis and characterization of new cardo poly(bisbenzoxazole)s containing fluorenylidene unit [J].Eur Polym J,2009,45(11):3187-3195.
[6] Sheng Shouri,Ge Weiwei,Huang Zhenzhong,et al.Synthesis and characteriaion of novel soluble cardo poly(arylene ether ketone)s containing xanthene structures [J].J Appl Polym Sci,2009,114(1):570-576.
[7] 李小青,杜晓华,郑鹛,等.绿色硝化反应的研究进展 [J].化工进展,2005,24(10):1073-1078.
[8] 姚蒙正,张若蘅.芳香族硝基化合物还原反应的若干进展 [J].化工进展,1984,1(4):19-25.
[9] 吕荣文,张竹霞,高昆玉.芳硝基物的水合肼催化还原研究进展 [J].染料与染色,2003,40(3):160-163.
[10] 贾志刚,李方实.液相催化加氢法制取芳胺的研究进展 [J].化工时刊,2004,1(18):1-4.

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备注/Memo

备注/Memo:
国家自然科学基金(21064003,51163008);江西省主要学科学术和技术带头人培养计划(20113BCB22012);江西省自然科学基金(20114BAB203014,20132BAB206031)
更新日期/Last Update: 1900-01-01