Pd-Fe/TiO_2催化硝基苯和醇羰基化合成苯氨基甲酸酯

Synthesis of Phenyl Carbamates by Carbonylation of Nitrobenzene with Alcohols over Pd-Fe/TiO_2 Catalyst

以Pd-Fe/TiO2为催化剂,硝基苯与醇或酚进行羰基化反应合成苯氨基甲酸酯,考察了反应条件和不同反应底物对羰基化反应的影响。结果发现Pd-Fe/TiO2催化剂对羰基化反应具有较好的催化活性,在硝基苯20 mmol,醇或酚21 mmol,Pd和Fe负载量分别为0.3%和0.1%,催化剂用量96 mg,乙腈20 mL,CO压力0.1 MPa,30℃反应3 h的条件下,硝基苯和醇或酚能顺利进行羰基化反应,以57.3%~96.8%的收率得到相应的苯氨基甲酸酯。催化剂重复使用8次,催化活性无明显下降。

Phenyl carbamates were synthezed by carbonylation of nitrobenzene with alcohols or phenols and carbon monoxide in the presence of Pd-Fe/TiO2 catalyst.The effects of reaction conditions and various substrates on the yield of phenyl carbamates were investigated.It was found that Pd-Fe/TiO2 catalyst showed high activity to carbonylation reactions.Mediated by Pd-Fe/TiO2 catalyst,the carbonylation reactions of some substrates can proceed well to phenyl carbamates in 57.3%~96.8% yield under the conditions of nitrobenzene 20 mmol,alcohol or phenol 21 mmol,mass fraction of Pd 0.3%,mass fraction of Fe 0.1%,catalyst dosage 96 mg,CH3CN 20 mL,CO pressure 0.1 MPa,reaction temperature 30 ℃,and reaction time 3 h.The catalyst can be reused at least eight times without significant decrease in activity.