高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (6): 894.

• 论文 • 上一篇    下一篇

Ru3(CO)9(TPPTS)3催化的水/有机两相芳香硝基化合物CO选择性还原的研究

梅建庭, 蒋景阳, 肖启明, 李亚明, 金子林   

  1. 大连理工大学精细化工国家重点实验室, 大连 116012
  • 收稿日期:1999-08-10 出版日期:2000-06-24 发布日期:2000-06-24
  • 通讯作者: 蒋景阳(1959年出生),男,博士,副教授,从事均相催化研究.
  • 基金资助:

    国家自然科学基金(批准号:29876004);教育部博士点科研基金

Studies of CO Selective Reduction of Aromatic Nitro Compounds in Water/Organic Phases by Using Ru3(CO)9(TPPTS)3

MEI Jian-Ting, JIANG Jing-Yang, XIAO Qi-Ming, LI Ya-Ming, JIN Zi-Lin   

  1. State Key Laboratory of Fine Chemicals, Dalian University of Technology, Dalian 116012, China
  • Received:1999-08-10 Online:2000-06-24 Published:2000-06-24

摘要: 将水溶性膦/钌配合物Ru3(CO)9(TPPTS)3(TPPTS:三苯基膦三-间磺酸钠)用于以CO为还原剂的水/有机两相芳香硝基化合物选择还原为芳胺的反应,发现相转移催化剂对反应有明显的促进作用,其中以添加十六烷基三甲基溴化铵(CTAB)的效果最好.以邻氯硝基苯为底物考察了相转移催化剂浓度、NaOH浓度、反应温度、压力等对反应转化率和选择性的影响.当反应条件为120℃,4MPa,3mol/LNaOH时,反应8h,邻氯硝基苯的转化率和邻氯苯胺的选择性均可达到99.9%.而且对含有羰基、氰基的芳香硝基化合物也有很高的活性和选择性.催化剂循环3次后,邻氯硝基苯的转化率和邻氯苯胺的收率仍可达到92%.

关键词: 水溶性膦/钌配合物, 水/有机两相催化, 芳香硝基化合物, CO选择性还原

Abstract: Ru3(CO)9(TPPTS)3 was used in the selective reduction of aromatic nitro compounds under COatmosphere in water/organic biphase system. It was found that the reaction was accelerated obviously by phase-transfer catalysts and the cetyltrimethylammonium bromide(CTAB) is the best one among them. Using o-ClC6H4NO2 as a reactant, the influences of the concentration of CTAB, the concentration of NaOH, reaction temperature and COpressure on the catalytic properties of Ru3(CO)9(TPPTS)3 were studied. Under the conditions of 120 ℃, pco =4 MPa, 3 mol/L NaOH, 8 h, both the conversions of o-ClC6H4NO2 and the selectivity of o-ClC6H4NH2 were 99.9%. The reductions proceeded with a markable activity and selectivity toward aromatic nitro group as C-O, C-Ngroups present in the substrate. After 3 times recycle of the catalyst the conversion of o-ClC6H4NO2 and the yield of o-ClC6H4NH2 were more than 92%.

Key words: Water-soluble phosphine ruthenium complex, Water/organic phase transfer catalysis, Aromatic nitro compounds, CO selective reduction

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