相转移催化法合成对硝基苯苄醚
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摘要
以对硝基苯酚、溴化苄为主要反应原料,在氢氧化钠存在下,用相转移催化剂在水相中催化合成了对硝基苯苄醚。研究表明,反应最佳条件:对硝基苯酚∶氢氧化钠∶溴化苄(摩尔比)=1.0∶1.15∶1.0,催化剂用量为3 g/mol对硝基苯酚,水的用量为3 000 m L/mol对硝基苯酚,在90℃下回流反应2.5 h,产物平均收率89.7%。该反应条件温和,时间短,操作简单,污染少,具有潜在应用前景。
With nitro phenol and benzyl bromide as the main raw material, the synthesis of nitrobenzene benzyl ether was studied in the presence of sodium hydroxide, using phase transfer catalyst in the water phase catalytic. Studies have shown that the optimum conditions: Under the optimal conditions: with the ratio of nitrophenol, base, and benzyl bromide(mole ratio)=1.0∶1.15∶1.0, catalyst 0.03 g, the amount of water for 30 m L at 90℃ within 2.5 h, the product yield up to 89.7%. The reaction with this method is moderate, short time, simple operation and less pollution.
With nitro phenol and benzyl bromide as the main raw material, the synthesis of nitrobenzene benzyl ether was studied in the presence of sodium hydroxide, using phase transfer catalyst in the water phase catalytic. Studies have shown that the optimum conditions: Under the optimal conditions: with the ratio of nitrophenol, base, and benzyl bromide(mole ratio)=1.0∶1.15∶1.0, catalyst 0.03 g, the amount of water for 30 m L at 90℃ within 2.5 h, the product yield up to 89.7%. The reaction with this method is moderate, short time, simple operation and less pollution.
引文
[1]万有志,张小强,范慧. 2,4-二硝基苯苄醚合成改进及表征[J].化学试剂, 2005, 27(5):303-304.
[2] Buchi G., Foulkes D M., Kurono M,et al. The total synthesis of racemic aflatoxim B[J]. J. Am. Chem. Soc.,1967, 89(25):6745-6749.
[3]樊能廷.有机合成事典[M].北京:北京理工大学出版社,1992:270.
[4]实用精细化学品手册编写组.实用精细化学品手册(下)[M].北京:化学工业出版社, 1996:1832.
[5]何伟明,翁志强.三氟甲基芳基硫醚的合成[J].化学进展, 2013,25(7):1071-1078.
[6]吴赛苏,倪秀琴,姜小红.对苯二酚二苯醚合成的新工艺[J].化学世界, 2001(9):472-475.
[7]李军,高爽,奚祖威.反应控制相转移催化研究的进展[J].催化学报,2010, 31(8):895-911.
[8]曲荣君,孙昌梅,王春华,等.相转移催化在高分子化合物合成中的应用[J].催化学报,2003,24(9):716-724.
[9]殷伟芬,辛淮生.羟基保护基MEMCIR的合成研究[J].精细与专用化学品, 2003, 15(6):19-20.
[10]李丕高,刘彦利.微波辐射法合成对硝基苯苄醚[J].石油化工,2006, 35(8):754-756.
[2] Buchi G., Foulkes D M., Kurono M,et al. The total synthesis of racemic aflatoxim B[J]. J. Am. Chem. Soc.,1967, 89(25):6745-6749.
[3]樊能廷.有机合成事典[M].北京:北京理工大学出版社,1992:270.
[4]实用精细化学品手册编写组.实用精细化学品手册(下)[M].北京:化学工业出版社, 1996:1832.
[5]何伟明,翁志强.三氟甲基芳基硫醚的合成[J].化学进展, 2013,25(7):1071-1078.
[6]吴赛苏,倪秀琴,姜小红.对苯二酚二苯醚合成的新工艺[J].化学世界, 2001(9):472-475.
[7]李军,高爽,奚祖威.反应控制相转移催化研究的进展[J].催化学报,2010, 31(8):895-911.
[8]曲荣君,孙昌梅,王春华,等.相转移催化在高分子化合物合成中的应用[J].催化学报,2003,24(9):716-724.
[9]殷伟芬,辛淮生.羟基保护基MEMCIR的合成研究[J].精细与专用化学品, 2003, 15(6):19-20.
[10]李丕高,刘彦利.微波辐射法合成对硝基苯苄醚[J].石油化工,2006, 35(8):754-756.