The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been conf...The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been confirmed by IR, 1H NMR, 13C NMR, LC-MS （ESI） and single-crystal X-ray diffraction. （R）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate crystallizes in monoclinic, space group P21/c with a = 11.867（2）, b = 8.4087（2）, c = 14.325（6） A^°, β = 117.59（2）°, Z = 4, V = 1266.9（6） A^°3, Dc = 1.307 g/cm^3, F（000） = 528, μ（MoKα） = 0.097 mm-1, R = 0.0453 and wR = 0.1237; （S）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate belongs to the triclinic system, space group P with a = 8.2647（17）, b = 8.7034（17）, c = 9.5479（19） A^°, α = 105.33（3）, β = 100.95（3）, γ = 105.14（3）°, Z = 2, V = 614.1（2） A^°3, Dc = 1.348 g/cm^3, F（000） = 264, μ（MoKα） = 0.10 mm-1, R = 0.0613 and wR = 0.1037. Both of the molecules prefer to form crystal packing through C–H…O hydrogen bonds.展开更多
This report describes triethylammonium acetate （TEAA） ionic liquid catalyzed one pot synthesis of 6-amino-4-aryl-5-cyano-3- methyl-1-phenyl-1,4-dihydropyrano [2,3-c]pyrazoles by the reaction of aromatic aldehyde, ma...This report describes triethylammonium acetate （TEAA） ionic liquid catalyzed one pot synthesis of 6-amino-4-aryl-5-cyano-3- methyl-1-phenyl-1,4-dihydropyrano [2,3-c]pyrazoles by the reaction of aromatic aldehyde, malononitrile and 3-methyl-1-phenyl-2- pyrazolin-5-one at room temperature. TEAA plays dual role as reaction media and catalyst. It can also be easily recovered and reused in several runs. TEAA provides greener reaction protocol to present methodology which obviates the need of organic solvents, expensive and toxic catalyst.展开更多
A series of 1,4-dihydropyridines have been prepared by a one-pot condensation of aldehydes,ethyl acetoacetate,and ammonium acetate in the presence of a heterogeneous catalyst silica sulfuric acid at room temperature u...A series of 1,4-dihydropyridines have been prepared by a one-pot condensation of aldehydes,ethyl acetoacetate,and ammonium acetate in the presence of a heterogeneous catalyst silica sulfuric acid at room temperature under solvent-free condition. This new protocol has the advantage of short reaction time and excellent yields,and is an environmentally benign route to the synthesis of 1,4-dihydropyridines.展开更多
The transesterification of diphenyl carbonate （DPC） with 1,4-butyldiol （BD） was kinetically investigated in the presence of lithium acetate catalyst at 465 K.The reaction was followed by the measurement of the qua...The transesterification of diphenyl carbonate （DPC） with 1,4-butyldiol （BD） was kinetically investigated in the presence of lithium acetate catalyst at 465 K.The reaction was followed by the measurement of the quantity of phenol which was distilled from the reactor.The experiments supported the assumption that the phenyl ester groups in DPC and phenyl hdroxybutyl carbonate （PHBH） had the same reactivity,and the transesterification obeyed first-order kinetics with respect to DPC and BD,and a rate equation was derived.The reaction rate was found to be first order with respect to the catalyst concentration as well.When those data were incorporated in the rate equation,excellent agreement between calculated values and the observed ones was recognized over a wide range.展开更多
A new lanthanide coordination polymer, [Dy（OAc）（BDC）]n 1 （OAc = acetate, BDC = 1,4-benzenediacarboxylate）, has been synthesized under hydrothermal conditions. Single-crystal X-ray diffraction analysis reveals th...A new lanthanide coordination polymer, [Dy（OAc）（BDC）]n 1 （OAc = acetate, BDC = 1,4-benzenediacarboxylate）, has been synthesized under hydrothermal conditions. Single-crystal X-ray diffraction analysis reveals that complex 1 has infinite zigzag Dy-OAc chains, which are further connected by BDC to form a 3D metal-organic framework. According to topology analysis, this framework can be characterized as （4,6）-connected （3.4.54）（32.4.56.66） net that has never been reported before. Crystal structure for 1： space group Pbca, a = 13.314（3）, b = 8.0269（18）, c = 20.275（5）A, V= 2166.8（9）A3, C10H7O6Dy, Mr = 385.66, Z= 8, Dc = 2.364 g/cm^3, μ= 6.910 mm^-1, F（000） = 1448, the final R = 0.0181 and wR = 0.0520.展开更多
Some 2 (2 chloro ethoxy) acetates were prepared by the reaction of 2 oxo 1,4 dixane with alcohol and thionyl chloride.Some reactions of ethyl 2 (2 chloro ethoxy) acetate were studied.2 Oxo 1,4 dixane was obtained rene...Some 2 (2 chloro ethoxy) acetates were prepared by the reaction of 2 oxo 1,4 dixane with alcohol and thionyl chloride.Some reactions of ethyl 2 (2 chloro ethoxy) acetate were studied.2 Oxo 1,4 dixane was obtained renewably by the reaction of ethyl 2 (2 chloro ethoxy) acetate base catalyzed hydrolysis.Under the condition of acid catalyzed hydrolysis,2 (2 chloro ethoxy) acetic acid was obtained.Using IR, 1HNMR and elemental analysis characterized these compounds that mentioned above using MS to confirme some compounds.展开更多
High-molecular-weight aliphatic polycarbonates（APCs） were synthesized through a two-step transesterification process under solvent-free conditions. Oligomers with equal numbers of hydroxyl and phenyl carbonate termi...High-molecular-weight aliphatic polycarbonates（APCs） were synthesized through a two-step transesterification process under solvent-free conditions. Oligomers with equal numbers of hydroxyl and phenyl carbonate terminal groups could be easily controlled by using equimolar amounts of diphenyl carbonate（DPC） and aliphatic diols as feedstocks in the first step. In the second step, the high-molecular-weight APCs can be obtained by connecting -OH with -OC（O）OC6H5 end-group upon removing the generated phenol at reduced pressure. Mg（OAc）2 was found to be the best catalyst for this process among the screened catalysts, which gave the poly（l,4-butylene carbonate）（PBC） a weight-average molecular weight（Mw） of 148600 and a yield of 84.8% under its suitable reaction conditions. In addition, based on the results of X-ray diffraction（XRD）, scanning electron microscopy（SEM） and fourier transform infrared spectroscopy（FTIR）, a possible reaction mechanism over Mg（OAe）2 was proposed for APCs synthesis.展开更多
基金supported by the National Natural Science Foundation of China(No.31572042)Natural Science Foundation of Heilongjiang Province(B201303)the Research Science Foundation in Technology Innovation of Harbin(No.2015RAYXJ010)
文摘The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been confirmed by IR, 1H NMR, 13C NMR, LC-MS （ESI） and single-crystal X-ray diffraction. （R）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate crystallizes in monoclinic, space group P21/c with a = 11.867（2）, b = 8.4087（2）, c = 14.325（6） A^°, β = 117.59（2）°, Z = 4, V = 1266.9（6） A^°3, Dc = 1.307 g/cm^3, F（000） = 528, μ（MoKα） = 0.097 mm-1, R = 0.0453 and wR = 0.1237; （S）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate belongs to the triclinic system, space group P with a = 8.2647（17）, b = 8.7034（17）, c = 9.5479（19） A^°, α = 105.33（3）, β = 100.95（3）, γ = 105.14（3）°, Z = 2, V = 614.1（2） A^°3, Dc = 1.348 g/cm^3, F（000） = 264, μ（MoKα） = 0.10 mm-1, R = 0.0613 and wR = 0.1037. Both of the molecules prefer to form crystal packing through C–H…O hydrogen bonds.
文摘This report describes triethylammonium acetate （TEAA） ionic liquid catalyzed one pot synthesis of 6-amino-4-aryl-5-cyano-3- methyl-1-phenyl-1,4-dihydropyrano [2,3-c]pyrazoles by the reaction of aromatic aldehyde, malononitrile and 3-methyl-1-phenyl-2- pyrazolin-5-one at room temperature. TEAA plays dual role as reaction media and catalyst. It can also be easily recovered and reused in several runs. TEAA provides greener reaction protocol to present methodology which obviates the need of organic solvents, expensive and toxic catalyst.
文摘A series of 1,4-dihydropyridines have been prepared by a one-pot condensation of aldehydes,ethyl acetoacetate,and ammonium acetate in the presence of a heterogeneous catalyst silica sulfuric acid at room temperature under solvent-free condition. This new protocol has the advantage of short reaction time and excellent yields,and is an environmentally benign route to the synthesis of 1,4-dihydropyridines.
基金supported by the Key Projects in the National Science & Technology Pillar Program during the Eleventh Five-Year Plan Period(2006BAE02B03)
文摘The transesterification of diphenyl carbonate （DPC） with 1,4-butyldiol （BD） was kinetically investigated in the presence of lithium acetate catalyst at 465 K.The reaction was followed by the measurement of the quantity of phenol which was distilled from the reactor.The experiments supported the assumption that the phenyl ester groups in DPC and phenyl hdroxybutyl carbonate （PHBH） had the same reactivity,and the transesterification obeyed first-order kinetics with respect to DPC and BD,and a rate equation was derived.The reaction rate was found to be first order with respect to the catalyst concentration as well.When those data were incorporated in the rate equation,excellent agreement between calculated values and the observed ones was recognized over a wide range.
基金the State Key Basic Research and Development Plan of China (2007CB815302)the Chinese Academy of Sciences (KJCX2-YW-M05)+3 种基金the NSF (E0620005) of Fujian Provincethe Major Special Foundation of Fujian Province (2005HZ1027, 2005HZ01-1)the Fund of Fujian Key Laboratory of Nanomaterials (2006L2005)the Knowledge Innovation Program of the Chinese Academy of Sciences
文摘A new lanthanide coordination polymer, [Dy（OAc）（BDC）]n 1 （OAc = acetate, BDC = 1,4-benzenediacarboxylate）, has been synthesized under hydrothermal conditions. Single-crystal X-ray diffraction analysis reveals that complex 1 has infinite zigzag Dy-OAc chains, which are further connected by BDC to form a 3D metal-organic framework. According to topology analysis, this framework can be characterized as （4,6）-connected （3.4.54）（32.4.56.66） net that has never been reported before. Crystal structure for 1： space group Pbca, a = 13.314（3）, b = 8.0269（18）, c = 20.275（5）A, V= 2166.8（9）A3, C10H7O6Dy, Mr = 385.66, Z= 8, Dc = 2.364 g/cm^3, μ= 6.910 mm^-1, F（000） = 1448, the final R = 0.0181 and wR = 0.0520.
文摘Some 2 (2 chloro ethoxy) acetates were prepared by the reaction of 2 oxo 1,4 dixane with alcohol and thionyl chloride.Some reactions of ethyl 2 (2 chloro ethoxy) acetate were studied.2 Oxo 1,4 dixane was obtained renewably by the reaction of ethyl 2 (2 chloro ethoxy) acetate base catalyzed hydrolysis.Under the condition of acid catalyzed hydrolysis,2 (2 chloro ethoxy) acetic acid was obtained.Using IR, 1HNMR and elemental analysis characterized these compounds that mentioned above using MS to confirme some compounds.
文摘High-molecular-weight aliphatic polycarbonates（APCs） were synthesized through a two-step transesterification process under solvent-free conditions. Oligomers with equal numbers of hydroxyl and phenyl carbonate terminal groups could be easily controlled by using equimolar amounts of diphenyl carbonate（DPC） and aliphatic diols as feedstocks in the first step. In the second step, the high-molecular-weight APCs can be obtained by connecting -OH with -OC（O）OC6H5 end-group upon removing the generated phenol at reduced pressure. Mg（OAc）2 was found to be the best catalyst for this process among the screened catalysts, which gave the poly（l,4-butylene carbonate）（PBC） a weight-average molecular weight（Mw） of 148600 and a yield of 84.8% under its suitable reaction conditions. In addition, based on the results of X-ray diffraction（XRD）, scanning electron microscopy（SEM） and fourier transform infrared spectroscopy（FTIR）, a possible reaction mechanism over Mg（OAe）2 was proposed for APCs synthesis.
