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- 2014
9,9-二(3-氨基-4-羟基苯基)?愣值暮铣捎氡碚?
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Abstract:
将9,9-二(4-羟基苯基)?愣钟胫柿颗ǘ任?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)?愣郑?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)?愣郑?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.
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