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有机化学
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有机化学 ›› 2010, Vol. 30 ›› Issue (06): 843-848. 上一篇    下一篇

研究论文

TiO2负载Pd-Fe催化氟代硝基苯羰基化合成氨基甲酸酯

刘长春*，卢卫平，颜延宁   

  1. 江苏食品职业技术学院生物化工系 淮安 223003
  • 收稿日期:2009-08-04 修回日期:2009-11-27 发布日期:2010-01-15
  • 通讯作者: 刘长春 E-mail:ccl67@126.com

Synthesis of Carbamates by Carbonylation of Floronitrobenzenes over TiO2 Supported Pd-Fe Catalyst

LIU Chang-Chun, LU Wei-Ping, YAN Yan-Ning   

  1. Department of Biochemical Engineering, Jiangsu Food Science College, Huai′an 223003
  • Received:2009-08-04 Revised:2009-11-27 Published:2010-01-15

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以TiO2负载Pd-Fe作催化剂, 研究了氟代硝基苯的羰基化反应. 结果表明, 在TiO2负载Pd-Fe催化剂的作用下, 不同的氟代硝基苯和醇或酚在常温常压下顺利进行羰基化反应, 大多数反应以较高的转化率和选择性得到氨基甲酸酯. Pd和Fe负载量、催化剂用量和反应温度等对羰基化反应有一定的影响, 优化反应条件为: 氟代硝基苯0.01 mol, 醇或酚0.01 mol, w(Pd)＝0.3%, w(Fe)＝0.1%, 催化剂52.6 mg, 乙腈10 mL, CO 0.1 MPa, 20 ℃, 反应时间3～9 h. 催化剂在反应结束后经简单处理可以重复使用.

关键词: 负载钯铁催化剂, 羰基化, 氨基甲酸酯, 氟代硝基苯

Carbonylation of fluoronitrobenzenes with alcohol or phenol to carbamates over TiO2 supported Pd-Fe catalyst was studied. Mediated by TiO2 supported Pd-Fe catalyst, different fluoronitrobenzenes reacted readily with alcohols or phenol and carbon monoxide to afford carbamates under room temperature and atmospheric pressure. The results show that the reaction can proceed well to carbamates in good conversion and high selectivity. Pd and Fe loading, catalyst dosage and reaction temperature affect the conversion and selectivity of carbonylation of fluoronitrobenzene over TiO2 supported Pd-Fe catalyst. The optimal reaction conditions are that fluoronitrobenzene 0.01 mol, alcohol or phenol 0.01 mol, mass fraction of Pd 0.3%, mass fraction of Fe 0.1%, catalyst dosage 52.6 mg, CH3CN 10 mL, CO 0.1 MPa, reaction temperature 20 ℃, and reaction time 3～9 h. The catalyst can be easily recovered and reused.

Key words: supported palladium-iron catalyst, carbonylation, carbamate, fluoronitrobenzene

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