引用本文:
张前锋, 唐安斌, 黄杰, 马寒冰, 杨玉川. 双(3-氨基-4-羟基苯基)双酚醚类化合物的合成[J]. 应用化学,
2013, 30(9): 986-992.
doi:
10.3724/SP.J.1095.2013.20501
Citation: ZHANG Qianfeng, TANG Anbin, HUANG Jie, MA Hanbing, YANG Yuchuan. Synthesis of Bis(3-amino-4-hydroxyphenyl) Bisphenol Ether[J]. Chinese Journal of Applied Chemistry, 2013, 30(9): 986-992. doi: 10.3724/SP.J.1095.2013.20501
Citation: ZHANG Qianfeng, TANG Anbin, HUANG Jie, MA Hanbing, YANG Yuchuan. Synthesis of Bis(3-amino-4-hydroxyphenyl) Bisphenol Ether[J]. Chinese Journal of Applied Chemistry, 2013, 30(9): 986-992. doi: 10.3724/SP.J.1095.2013.20501
双(3-氨基-4-羟基苯基)双酚醚类化合物的合成
摘要:
以双酚化合物及对卤苯酚为起始原料,经用苄基保护、乌尔曼成醚、选择性硝化和还原脱保护4步反应,合成了具有双酚芳香醚结构的4个新型聚苯并□唑单体:双(3-氨基-4-羟基苯基)双酚醚类化合物的盐酸盐。确定了乌尔曼成醚反应的最佳工艺条件,证明硝化反应只发生在对卤苯酚苄保护基的邻位,改进了还原脱保护反应的成盐及后处理条件,提高了产物的质量和收率,4步反应总收率可达54.0%。采用红外光谱、核磁共振H谱和高分辨质谱表征了每步产物的化学结构。
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关键词:
- 聚苯并!唑单体
- / 乌尔曼反应
- / 双氨基羟基苯基双酚醚
- / 合成
English
Synthesis of Bis(3-amino-4-hydroxyphenyl) Bisphenol Ether
Abstract:
Four monomers of polybenzoxazole having the structure of bisphenol aromatic ether,bis(3-amino-hydroxyphenyl) bisphenol ether,were prepared from bisphenols and 4-chloro(or bromo)-phenol by successive 4 steps of synthetic routes including benzyl protection,Ullmann reaction, selective nitrification and reduction-deprotection. The effect of reaction conditions on the Ullmann reaction was investigated. The high region selection of the nitrification is confirmed. The process of after-treatment of the reduction-deprotection was optimized and the quality and yield of the product were improved. The total yield of 4 steps reaction can reach up to 54.0%. The target compound and its intermediates were characterized by means of IR,1H NMR and HRMS.
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