The title compound 4-(3,4-methylenedioxylphenyl)-6-methyl-5-ethoxycaronyl-3,4- dihydropyrimidin-2(H)-one (C15H16N2O5) has been synthesized and determined by single-crystal X-ray diffraction. The crystal is of triclini...The title compound 4-(3,4-methylenedioxylphenyl)-6-methyl-5-ethoxycaronyl-3,4- dihydropyrimidin-2(H)-one (C15H16N2O5) has been synthesized and determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 7.580(1), b = 7.920(2), c = 13.168(4) ? a = 96.44(2), b = 96.71(2), g = 109.81(2), V = 728.8(3) 3, Z = 2, Mr = 304.30, Dc = 1.387 g/cm3, F(000) = 320, m(MoKa) = 0.105 mm-1 (l = 0.71073 ?, R = 0.0446 and wR = 0.1205. In the molecule the pyrimidine ring adopts a boat conformation.展开更多
A series of Biginelli compounds was synthesized using TsOH as a catalyst under microwave irradiation. This simple method provided the title compounds in 86%-98% yields by the reaction of aromatic aldehydes with 1,3 c...A series of Biginelli compounds was synthesized using TsOH as a catalyst under microwave irradiation. This simple method provided the title compounds in 86%-98% yields by the reaction of aromatic aldehydes with 1,3 carbonyl compound and urea. The structure of 4o was determined by single crystal X ray diffraction analysis.展开更多
通过1-乙基-3-甲基咪唑硫酸乙酯离子液体(EMIES)和对甲苯磺酸(p-TsOH)的混合物制备EMIES/p-TsOH型低共熔溶剂。其结构特征通过红外光谱、氢谱和热重技术进行了分析。并以EMIES/p-TsOH作为催化剂与萃取剂,H2O2作为氧化剂研究了其对模拟...通过1-乙基-3-甲基咪唑硫酸乙酯离子液体(EMIES)和对甲苯磺酸(p-TsOH)的混合物制备EMIES/p-TsOH型低共熔溶剂。其结构特征通过红外光谱、氢谱和热重技术进行了分析。并以EMIES/p-TsOH作为催化剂与萃取剂,H2O2作为氧化剂研究了其对模拟油中的硫化物的脱除性能。考察了反应温度、n(H2O2)/n(S)比、低共熔溶剂加入量及硫化物类型对脱硫效果的影响。在最佳的条件下,模拟油中二苯并噻吩(DBT)、4,6-二甲基二苯并噻吩(4,6-DMDBT)和苯并噻吩(BT)的脱除率分别为96.2%、92.2%和88.8%。经过五次循环使用后,DBT的脱除率仍达到93.6%。对该脱硫体系进行了动力学分析,其表观活化能为66.4 k J/mol。展开更多
通过简单加热氯代正丁基吡啶([C_4Pyr]Cl)和对甲苯磺酸(TsOH)的混合物制备了[C_4Pyr]Cl/nTsOH,(n=0.1,0.2,0.3)型低共熔溶剂。以[C_4Pyr]Cl/nTsOH为催化剂和萃取剂,H_2O_2为氧化剂组成萃取-催化氧化脱硫体系氧化脱除模拟油中的硫化物。...通过简单加热氯代正丁基吡啶([C_4Pyr]Cl)和对甲苯磺酸(TsOH)的混合物制备了[C_4Pyr]Cl/nTsOH,(n=0.1,0.2,0.3)型低共熔溶剂。以[C_4Pyr]Cl/nTsOH为催化剂和萃取剂,H_2O_2为氧化剂组成萃取-催化氧化脱硫体系氧化脱除模拟油中的硫化物。通过FTIR表征,确定[C_4Pyr]Cl/0.2TsOH的结构以及氧化产物,并考察了不同脱硫体系、n(TsOH)∶n([C_4Pyr]Cl)、低共熔溶剂加入量、反应温度、n(H_2O_2)∶n(二苯并噻吩)和含硫化物类型对脱硫效果的影响。实验结果表明,在低共熔溶剂[C_4Pyr]Cl/0.2TsOH加入量1.00 m L、反应温度50℃、n(H_2O_2)∶n(二苯并噻吩)=6、模拟油用量5 m L的反应条件下,[C_4Pyr]Cl/0.2TsOH对二苯并噻吩、4,6-二甲基二苯并噻吩和苯并噻吩的脱硫率分别达98.2%,96.0%,40.2%。由一级动力学方程和Arrhenius方程计算氧化脱除二苯并噻吩所需的表观活化能约为51.95 k J/mol。[C_4Pyr]Cl/0.2TsOH回收利用5次后,脱硫率仍不低于95.1%。展开更多
A facile synthesis of benzo[h]quinolines has been developed via improved Combes reaction. A combination of silica gel, p-toluenesulfonic acid and phosphorus pentoxide was utilized to promote the condensation of 1-naph...A facile synthesis of benzo[h]quinolines has been developed via improved Combes reaction. A combination of silica gel, p-toluenesulfonic acid and phosphorus pentoxide was utilized to promote the condensation of 1-naphthylamines with 1,3-diketones under solvent free conditions. In this case, silica gel was used as reaction media, p-toluenesulfonic acid and phosphorus pentoxide were acted as catalyst and dehydrating agent, respectively.展开更多
基金Supported by the National Natural Science Foundation of China (No. 20372057) Natural Science Foundation of Jiangsu Province (No. BK2001142) and the Natural Science Foundation of Jiangsu Education Department (No. 01KJB150008) and Jiangsu Provincial
文摘The title compound 4-(3,4-methylenedioxylphenyl)-6-methyl-5-ethoxycaronyl-3,4- dihydropyrimidin-2(H)-one (C15H16N2O5) has been synthesized and determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 7.580(1), b = 7.920(2), c = 13.168(4) ? a = 96.44(2), b = 96.71(2), g = 109.81(2), V = 728.8(3) 3, Z = 2, Mr = 304.30, Dc = 1.387 g/cm3, F(000) = 320, m(MoKa) = 0.105 mm-1 (l = 0.71073 ?, R = 0.0446 and wR = 0.1205. In the molecule the pyrimidine ring adopts a boat conformation.
基金ProjectsupportedbytheNaturalScienceFoundationofJiangsuProvince (No .BK2 0 0 114 2 )andtheNaturalScienceFoundationofJiang suEducationDepartment (No .0 1KJB15 0 0 0 8)andJiangsuProvinceKeyLaboratoryofChemical&EngineeringandTechnologyFounda tion (No .KJ
文摘A series of Biginelli compounds was synthesized using TsOH as a catalyst under microwave irradiation. This simple method provided the title compounds in 86%-98% yields by the reaction of aromatic aldehydes with 1,3 carbonyl compound and urea. The structure of 4o was determined by single crystal X ray diffraction analysis.
文摘通过1-乙基-3-甲基咪唑硫酸乙酯离子液体(EMIES)和对甲苯磺酸(p-TsOH)的混合物制备EMIES/p-TsOH型低共熔溶剂。其结构特征通过红外光谱、氢谱和热重技术进行了分析。并以EMIES/p-TsOH作为催化剂与萃取剂,H2O2作为氧化剂研究了其对模拟油中的硫化物的脱除性能。考察了反应温度、n(H2O2)/n(S)比、低共熔溶剂加入量及硫化物类型对脱硫效果的影响。在最佳的条件下,模拟油中二苯并噻吩(DBT)、4,6-二甲基二苯并噻吩(4,6-DMDBT)和苯并噻吩(BT)的脱除率分别为96.2%、92.2%和88.8%。经过五次循环使用后,DBT的脱除率仍达到93.6%。对该脱硫体系进行了动力学分析,其表观活化能为66.4 k J/mol。
文摘通过简单加热氯代正丁基吡啶([C_4Pyr]Cl)和对甲苯磺酸(TsOH)的混合物制备了[C_4Pyr]Cl/nTsOH,(n=0.1,0.2,0.3)型低共熔溶剂。以[C_4Pyr]Cl/nTsOH为催化剂和萃取剂,H_2O_2为氧化剂组成萃取-催化氧化脱硫体系氧化脱除模拟油中的硫化物。通过FTIR表征,确定[C_4Pyr]Cl/0.2TsOH的结构以及氧化产物,并考察了不同脱硫体系、n(TsOH)∶n([C_4Pyr]Cl)、低共熔溶剂加入量、反应温度、n(H_2O_2)∶n(二苯并噻吩)和含硫化物类型对脱硫效果的影响。实验结果表明,在低共熔溶剂[C_4Pyr]Cl/0.2TsOH加入量1.00 m L、反应温度50℃、n(H_2O_2)∶n(二苯并噻吩)=6、模拟油用量5 m L的反应条件下,[C_4Pyr]Cl/0.2TsOH对二苯并噻吩、4,6-二甲基二苯并噻吩和苯并噻吩的脱硫率分别达98.2%,96.0%,40.2%。由一级动力学方程和Arrhenius方程计算氧化脱除二苯并噻吩所需的表观活化能约为51.95 k J/mol。[C_4Pyr]Cl/0.2TsOH回收利用5次后,脱硫率仍不低于95.1%。
文摘A facile synthesis of benzo[h]quinolines has been developed via improved Combes reaction. A combination of silica gel, p-toluenesulfonic acid and phosphorus pentoxide was utilized to promote the condensation of 1-naphthylamines with 1,3-diketones under solvent free conditions. In this case, silica gel was used as reaction media, p-toluenesulfonic acid and phosphorus pentoxide were acted as catalyst and dehydrating agent, respectively.
