采用溶胶-凝胶法制备H3PW6Mo6O40/SiO2催化剂,以苯甲醛,乙酰乙酸乙酯和尿素为原料,无水乙醇为溶剂催化合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮,研究结果表明:反应物的摩尔比、反应温度、催化剂用量和反应时间是影响4-苯基-6...采用溶胶-凝胶法制备H3PW6Mo6O40/SiO2催化剂,以苯甲醛,乙酰乙酸乙酯和尿素为原料,无水乙醇为溶剂催化合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮,研究结果表明:反应物的摩尔比、反应温度、催化剂用量和反应时间是影响4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮合成收率的重要因素.当n(苯甲醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1.0∶1.2∶1.5,反应温度为90℃,催化剂的用量占反应物料总质量的1.5%,反应时间为75min时,产品收率可达70.3%.通过熔点、IR、1 H NMR和MS对合成目标化合物进行了表征确认.展开更多
A new environmental friendly catalyst, HaSiWrMo6O40/PAn was prepared and identified by means of FT-IR, XRD and TG/DTA. The optimum conditions have been found, that was, mass ratio of m（PAn）： m（HaSiW6Mo6On.） was 1...A new environmental friendly catalyst, HaSiWrMo6O40/PAn was prepared and identified by means of FT-IR, XRD and TG/DTA. The optimum conditions have been found, that was, mass ratio of m（PAn）： m（HaSiW6Mo6On.） was 1：1.25, volume of methanol was 20 mL, and the reflux reaction time was 2h. The structural identity of Keggin units was preserved after the incorporation into polyaniline matrix. H4SiW6Mo6040/PAn was used as catalyst in catalytic synthesis of acetals and ketals. Effects of n（aldehyde（ketone ））： n（glycol）, catalyst dosage and reaction time on yield were investingated. Optimal conditions were： n（aldehyde（ketone））： n（glycol）=1.0： 1.5; mass fraction of catalyst to reactants, 0.5%; reaction time, 1.0 h and cyclohexane as water-stripped reagent, 15 mL. Under these conditions, yields of actels and ketals were 31.9%-91.6%.展开更多
文摘采用溶胶-凝胶法制备H3PW6Mo6O40/SiO2催化剂,以苯甲醛,乙酰乙酸乙酯和尿素为原料,无水乙醇为溶剂催化合成4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮,研究结果表明:反应物的摩尔比、反应温度、催化剂用量和反应时间是影响4-苯基-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮合成收率的重要因素.当n(苯甲醛)∶n(乙酰乙酸乙酯)∶n(尿素)=1.0∶1.2∶1.5,反应温度为90℃,催化剂的用量占反应物料总质量的1.5%,反应时间为75min时,产品收率可达70.3%.通过熔点、IR、1 H NMR和MS对合成目标化合物进行了表征确认.
文摘A new environmental friendly catalyst, HaSiWrMo6O40/PAn was prepared and identified by means of FT-IR, XRD and TG/DTA. The optimum conditions have been found, that was, mass ratio of m（PAn）： m（HaSiW6Mo6On.） was 1：1.25, volume of methanol was 20 mL, and the reflux reaction time was 2h. The structural identity of Keggin units was preserved after the incorporation into polyaniline matrix. H4SiW6Mo6040/PAn was used as catalyst in catalytic synthesis of acetals and ketals. Effects of n（aldehyde（ketone ））： n（glycol）, catalyst dosage and reaction time on yield were investingated. Optimal conditions were： n（aldehyde（ketone））： n（glycol）=1.0： 1.5; mass fraction of catalyst to reactants, 0.5%; reaction time, 1.0 h and cyclohexane as water-stripped reagent, 15 mL. Under these conditions, yields of actels and ketals were 31.9%-91.6%.
