H4SiW12O40／SiO2高效催化一锅法合成2-（1-苯胺基）苯甲基-环己酮

目的合成2-(1-苯胺基)苯甲基-环己酮。方法在室温条件下,采用溶胶凝胶法合成H_4SiW_(12)O_(40)/SiO_2催化剂,高效催化环己酮、苯甲醛和苯胺的Mannich反应合成2-(1-苯胺基)苯甲基-环己酮。结果在n(苯甲醛):n(环己酮):n(苯胺)=1.0∶1.8∶1.8,反应温度为20℃,催化剂的用量占反应物料总质量的10%,反应时间为23h的最佳条件下,2-(1-苯胺基)苯甲基-环己酮的收率可达77.5%。结论 H_4SiW_(12)O_(40)/SiO_2是合成2-(1-苯胺基)苯甲基-环己酮的优良催化剂,整个反应体系具有条件温和、操作简单、对环境友好和催化剂可重复回收利用等优点。

Efficient one-pot synthesis of 2-(1-anilino)benzyl-cyclohexanone with H4SiW12 O40/SiO2

Objective To synthesize 2-(1-anilino)benzyl-cyclohexanone.Methods A new environ-mental friendly catalyst,H4 SiW12 O40/SiO2 was prepared with sol-gel method.The catalyst exhibited excellent catalytic activities for the synthesis of 2-(1-anilino)benzyl-cyclohexanone via three-compo-nent Mannich reaction of aniline,benzaldehyde and cyclohexanone.Results The effects of reaction on the yield of 2-(1-anilino)benzyl-cyclohexanone were investigated and the optimum conditions were de-termined as follows:the molar ratio of benzaldehyde to cyclohexanone to aniline was n (benzaldehyde):n (cyclohexanone):n (aniline)= 1.0∶1.8∶1.8,reaction temperature was 20 ℃,the mass ratio of the catalyst to total reactant was 10%,and reaction time was 23 h,the yield of 2-(1-anilino)ben-zyl-cyclohexanone could reach 77.5%.Conclusion The results showed that the reaction catalyzed by H4 SiW12 O40/SiO2 has advantages of mild reaction conditions,simple operation,easy isolation and re-cyclable catalyst.