TiO_2负载Pd-Fe催化氟代硝基苯羰基化合成氨基甲酸酯

Synthesis of Carbamates by Carbonylation of Floronitrobenzenes over TiO_2 Supported Pd-Fe Catalyst

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0.01mol,醇或酚0.01mol,w(Pd)=0.3%,w(Fe)=0.1%,催化剂52.6mg,乙腈10mL,CO0.1MPa,20℃,反应时间3～9h.催化剂在反应结束后经简单处理可以重复使用.

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.