糠醛、乙酸酐为原料,用4-二甲氨基吡啶(DMAP)作催化剂,在吡啶存在下,经Perk in反应一步合成了α-呋喃丙烯酸。考察了原料配比、反应温度和时间以及吡啶和DMAP用量对产物收率的影响,优化的工艺条件为:n(糠醛)∶n(乙酸酐)∶n(DMAP)∶n(吡...糠醛、乙酸酐为原料,用4-二甲氨基吡啶(DMAP)作催化剂,在吡啶存在下,经Perk in反应一步合成了α-呋喃丙烯酸。考察了原料配比、反应温度和时间以及吡啶和DMAP用量对产物收率的影响,优化的工艺条件为:n(糠醛)∶n(乙酸酐)∶n(DMAP)∶n(吡啶)=1∶3∶0.05∶1,反应温度140℃,反应时间30 m in,产物最终收率可达89.2%。展开更多
以联苯为原料,经傅克酰化、溴代、格氏和氧化反应,制备了4-(4-乙酰基苯基)苯甲酸;以苯甲醚为原料经傅克酰化,醚解制备了4-乙酰基苯酚;两者再经酯化、还原、脱水反应,合成了一种新型的双官能团聚合物材料单体4-(4-乙烯基)苯基苯甲酸-(4-...以联苯为原料,经傅克酰化、溴代、格氏和氧化反应,制备了4-(4-乙酰基苯基)苯甲酸;以苯甲醚为原料经傅克酰化,醚解制备了4-乙酰基苯酚;两者再经酯化、还原、脱水反应,合成了一种新型的双官能团聚合物材料单体4-(4-乙烯基)苯基苯甲酸-(4-乙烯基)苯酯,基于联苯的总收率为7%～10%,其结构经1 H NMR和FT-IR确认,并用偏光显微镜和差示扫描量热仪对其液晶性进行了研究。展开更多
Herein,a DMAP-catalyzed[4+2]annulation ofα-substituted allenoates with arylazosulfones is reported,which affords facile access to tetrahydropyridazine derivative in synthetically useful yields.This reaction features ...Herein,a DMAP-catalyzed[4+2]annulation ofα-substituted allenoates with arylazosulfones is reported,which affords facile access to tetrahydropyridazine derivative in synthetically useful yields.This reaction features mild conditions and good functional group tolerance.Moreover,the resultant products can be readily transformed into pyridazin-3-one derivatives in the presence of DDQ.展开更多
文摘糠醛、乙酸酐为原料,用4-二甲氨基吡啶(DMAP)作催化剂,在吡啶存在下,经Perk in反应一步合成了α-呋喃丙烯酸。考察了原料配比、反应温度和时间以及吡啶和DMAP用量对产物收率的影响,优化的工艺条件为:n(糠醛)∶n(乙酸酐)∶n(DMAP)∶n(吡啶)=1∶3∶0.05∶1,反应温度140℃,反应时间30 m in,产物最终收率可达89.2%。
文摘以联苯为原料,经傅克酰化、溴代、格氏和氧化反应,制备了4-(4-乙酰基苯基)苯甲酸;以苯甲醚为原料经傅克酰化,醚解制备了4-乙酰基苯酚;两者再经酯化、还原、脱水反应,合成了一种新型的双官能团聚合物材料单体4-(4-乙烯基)苯基苯甲酸-(4-乙烯基)苯酯,基于联苯的总收率为7%～10%,其结构经1 H NMR和FT-IR确认,并用偏光显微镜和差示扫描量热仪对其液晶性进行了研究。
基金the Independent Research Foundation of Key Laboratory of Green and Precise Synthetic Chemistry and Applications in Huaibei Normal University,Ministry of Educationthe University Top Talents Academic Funding Project of Anhui Province(gxbjzD2021097)+1 种基金the Natural Science Foundation of Educational Committee from Anhui Province and Huaibei Normal University(KJ2020A0045,KJ2020A1199,KJ2020B01,2023ZK078,2023ZK079)the University Synergy Innovation Program of Anhui Province(GXXT-2020-078)for financial support of this work.
文摘Herein,a DMAP-catalyzed[4+2]annulation ofα-substituted allenoates with arylazosulfones is reported,which affords facile access to tetrahydropyridazine derivative in synthetically useful yields.This reaction features mild conditions and good functional group tolerance.Moreover,the resultant products can be readily transformed into pyridazin-3-one derivatives in the presence of DDQ.
