The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group C2/c with a=18.520(2),b=7.8910(1),c=21.728(3)?,β=104.77(1)°...The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group C2/c with a=18.520(2),b=7.8910(1),c=21.728(3)?,β=104.77(1)°,V=3070.4(7)?^3,Mr=303.31,Z=8,Dc=1.312g/cm^3,λ=0.71073?,μ(MoKα)=0.098mm^-1 and F(000)=1280.The structure was refined to R=0.0486 and wR=0.1287.There exist intermolecular hydrogen bonds in the crystal.展开更多
The title compound （C19H23NO3） was synthesized by the one-pot reaction ofp-methoxybenzaldehyde, Meldrum＇s acid, dimedone and CH3NH3Cl （NaOAc） in ethanol under microwave irradiation without catalyst and its crysta...The title compound （C19H23NO3） was synthesized by the one-pot reaction ofp-methoxybenzaldehyde, Meldrum＇s acid, dimedone and CH3NH3Cl （NaOAc） in ethanol under microwave irradiation without catalyst and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 8.7462（10）, b = 17.7367（19）, c = 11.5959（14） A, β = 110.981（3）°, V= 1679.6（3） A^3, Z = 4, Dc = 1.239 g/cm^3,μ（MoKa） = 0.083 mm^-1, F（000） = 672 and Mr = 313.38. The structure was refined to R = 0.0530 and wR = 0.1216. X-ray analysis reveals that the dihedral angle between plane 1 （N（1）, C（1）, C（2）, C（3）） and plane 2 （C（1）, C（2）, C（6）, C（7）, C（9）） is 3.64°, andt hat between plane 2 and plane 3 （C（11）～C（16）） is 85.33°.展开更多
The crystal structure N-methyl-9-(4-bromophenyl)-1,8-dioxo-1,2,3,4,5,6,7,8,9,10- decahydroacridine(C20H20BrNO2) was determined by single-crystal X-ray diffraction analysis. It belongs to P21/n space group, with a = ...The crystal structure N-methyl-9-(4-bromophenyl)-1,8-dioxo-1,2,3,4,5,6,7,8,9,10- decahydroacridine(C20H20BrNO2) was determined by single-crystal X-ray diffraction analysis. It belongs to P21/n space group, with a = 10.7999(18), b = 13.845(3), c = 11.4031(3) ?, β = 99.324(4)°, Dc = 1.525 g/cm3, Z = 4, λ = 0.71070 ?, μ(MoKα) = 2.455 mm-1, Mr = 386.28, V = 1682.5(5) ?3, F(000) = 792, the final R = 0.0463 and wR = 0.1053. In the crystal structure, the pyridine ring adopts a boat conformation, the two six-numbered rings fused with pyridine ring adopt twisting boat con- formation.展开更多
The N-cyclopropyl-9-(3,4-dicholophenyl)-1,2,3,4,5,6,7,8,9,10-decahydroacri- dine-1,8-dione was synthesized by the reaction of 1,3-cyclohexanedione, N-cyclopropylamine and 3,4-dicholoaldehyde in water and glycol under ...The N-cyclopropyl-9-(3,4-dicholophenyl)-1,2,3,4,5,6,7,8,9,10-decahydroacri- dine-1,8-dione was synthesized by the reaction of 1,3-cyclohexanedione, N-cyclopropylamine and 3,4-dicholoaldehyde in water and glycol under microwave irradiation. Its crystal structure was determined by single-crystal X-ray diffraction analysis. It possesses P212121 space group, with a = 9.9103(5), b = 13.3597(8), c = 14.5633(8) ?, V = 1928.16(18) ?3, Mr = 402.30, Z = 4, Dc = 1.386 g/cm3, λ = 0.7107 ?, μ(MoKα) = 0.354 mm?1 and F (000) = 840. The structure was refined to R = 0.0280 and wR = 0.0757. In the structure, the pyridine ring adopts a boat conformation.展开更多
The title compound 5-cyclopropyl-10-（4-fluorophenyl）-7,7-dimethyl-7,8-dihydro- 5H-indeno[1,2-b]quinolne-9,11（6H,10H）-dione was obtained by the reaction of 4-fluorobenzal- dehyde, 2H-indene-1,3-dione and 3-（cyclop...The title compound 5-cyclopropyl-10-（4-fluorophenyl）-7,7-dimethyl-7,8-dihydro- 5H-indeno[1,2-b]quinolne-9,11（6H,10H）-dione was obtained by the reaction of 4-fluorobenzal- dehyde, 2H-indene-1,3-dione and 3-（cyclopropylamino）-5,5-dimethylcyclohex-2-enone in the presence of acetic acid under microwave irradiation. Its structure was confirmed by IR and 1H- NMR spectra. The crystal is of monoclinic, space group P21/c with a = 14.138（3）, b = 8.952（2）, c = 17.140（3）A, β = 102.253（3）°, C27H24FNO2, Mr = 413.47, Z = 4, V = 2119.9（8）A^3, Dc = 1.296 g/cm^3, μ（MoKα） = 0.087 mm^-1, F（000） = 872, the final R = 0.0425 and wR = 0.0905 for 2336 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the pyridine ring adopts a boat conformation and the six-membered ring fused with it assumes a twist boat conformation.展开更多
The title compound (C25H24N4O3) has been prepared by the cyclocondensation of 5-amino-3-methyl-1-phenypyrazol, m-nitrobenaldehyde and dimedone in glycol under microwave irradiation without catalyst. The crystal stru...The title compound (C25H24N4O3) has been prepared by the cyclocondensation of 5-amino-3-methyl-1-phenypyrazol, m-nitrobenaldehyde and dimedone in glycol under microwave irradiation without catalyst. The crystal structure was determined by single-crystal X-ray diffraction to be orthorhombic, space group Pbca with a = 16.3331(10), b = 13.8329(9), c = 19.4163(12) ?, V = 4386.8(5) ?3, Z = 8, Dc = 1.298 g/cm3, μ = 0.087 mm-1, F(000) = 1808, Mr = 428.48, the final R = 0.0519 and wR = 0.1019. X-ray analysis revealed that the pyridine ring is of boat conformation and the six-membered ring fused with it adopts twist boat conformation.② Corresponding author. Tu Shu-Jiang, born in 1957, professor, majoring in the synthesis of organic and heterocycle compounds. E-mail: laotu2001@ 263.net展开更多
4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the cataly...4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the catalyst.Its structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic crystal system,P-1 space group,a=9.5470(19)?,b=13.637(3)?,c=16.029(3)?,α=75.33(3)°,β=83.62(3)°,γ=70.99(3)°,V=1097.8(7)s assembled into supramolecule structure by intermolecular hydrogen bonds.展开更多
Benzoxazinone usually exists in many kinds of plants.It is applied in prepharmacy synthesis,and bioactivity studies,and has been prepared from O-aminophenol and chrol-with alkine and solvent by refluxing for a long ti...Benzoxazinone usually exists in many kinds of plants.It is applied in prepharmacy synthesis,and bioactivity studies,and has been prepared from O-aminophenol and chrol-with alkine and solvent by refluxing for a long time.In this work,2,2’-diphenyl-1,4-benzoxazin-3(4H)-one was solvent-free synthesized under microwave irradiation.The configuration and conformation of the product were determined by 1H NMR,IR,MS,elementary analysis and X-ray crystal analysis.The results of X-ray crystal analysis show that the compound crystallizes in a triclinic system,space group %P%1,cell parameter %a%=0.840 7(1)nm,%b%=0.845 1(1)nm,%c%=2.254 1(3)nm,%α%=96.111(3)°,%β%=97.196(3)°,%γ%=90.229(3)°,%V%= 1^579 6(4)nm3,%Z%=4,%D%c =1.267 Mg/m3,%F%(000)= 632.0,%μ%= 0.08 mm-1.In the compound,oxazinone ring is shown chair conformation,two benzene rings is placed in two sides of oxazinone ring distortedly.In crystal state,a centrosymmetric dimmer is formed %via% hydrogen bonds generated from amides of two near molecules.The benzene rings in a same chemical environment are paralleled by a distance of 0.260 9 nm.It displays aromatic π-π stacking interactions.展开更多
基金Supported by the Natural Science Foundation of Jiangsu province(No.BK2001142)the Natural Science Foundation of Jiangsu Education Department(No.01KJB150008)
文摘The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction.The crystal is of monoclinic,space group C2/c with a=18.520(2),b=7.8910(1),c=21.728(3)?,β=104.77(1)°,V=3070.4(7)?^3,Mr=303.31,Z=8,Dc=1.312g/cm^3,λ=0.71073?,μ(MoKα)=0.098mm^-1 and F(000)=1280.The structure was refined to R=0.0486 and wR=0.1287.There exist intermolecular hydrogen bonds in the crystal.
基金The project was supported by the National Natural Science Foundation of China (No. 20372057), the Natural Science Foundation of Jiangsu Province (No. BK2001142), the Open Foundation of Key Laboratory of Organic Synthesis of Jiangsu Province, College of Chemistry and Chemical Engineering, Suzhou University (JSK 011) and the Key Lab of Biotechnology for Medicinal Plants of Jiangsu Province (01AXL 14)
文摘The title compound （C19H23NO3） was synthesized by the one-pot reaction ofp-methoxybenzaldehyde, Meldrum＇s acid, dimedone and CH3NH3Cl （NaOAc） in ethanol under microwave irradiation without catalyst and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 8.7462（10）, b = 17.7367（19）, c = 11.5959（14） A, β = 110.981（3）°, V= 1679.6（3） A^3, Z = 4, Dc = 1.239 g/cm^3,μ（MoKa） = 0.083 mm^-1, F（000） = 672 and Mr = 313.38. The structure was refined to R = 0.0530 and wR = 0.1216. X-ray analysis reveals that the dihedral angle between plane 1 （N（1）, C（1）, C（2）, C（3）） and plane 2 （C（1）, C（2）, C（6）, C（7）, C（9）） is 3.64°, andt hat between plane 2 and plane 3 （C（11）～C（16）） is 85.33°.
基金This work was supported by the National Natural Science Foundation of China (No. 20372057) Natural Science Foundation of Jiangsu Province (No. BK2001142) the Suzhou University Organic Synthesis Open Laboratory of Jiangsu Province (No. S81091 11) and the Key Lab of Biotechnology for Medicinal Plants of Jiangsu Province (No. 01AXL 14)
文摘The crystal structure N-methyl-9-(4-bromophenyl)-1,8-dioxo-1,2,3,4,5,6,7,8,9,10- decahydroacridine(C20H20BrNO2) was determined by single-crystal X-ray diffraction analysis. It belongs to P21/n space group, with a = 10.7999(18), b = 13.845(3), c = 11.4031(3) ?, β = 99.324(4)°, Dc = 1.525 g/cm3, Z = 4, λ = 0.71070 ?, μ(MoKα) = 2.455 mm-1, Mr = 386.28, V = 1682.5(5) ?3, F(000) = 792, the final R = 0.0463 and wR = 0.1053. In the crystal structure, the pyridine ring adopts a boat conformation, the two six-numbered rings fused with pyridine ring adopt twisting boat con- formation.
基金This work was supported by the National Natural Science Foundation of China (No. 20372057), the Natural Science Foundation of the Jiangsu Province (No. BK2001142), the Suzhou University Organic Syntheses Open Laboratory of Jiangsu Province (No. S8109111) and the Key Lab of Biotechnology for Medicinal Plants of Jiangsu Province (No. 01AXL 14)
文摘The N-cyclopropyl-9-(3,4-dicholophenyl)-1,2,3,4,5,6,7,8,9,10-decahydroacri- dine-1,8-dione was synthesized by the reaction of 1,3-cyclohexanedione, N-cyclopropylamine and 3,4-dicholoaldehyde in water and glycol under microwave irradiation. Its crystal structure was determined by single-crystal X-ray diffraction analysis. It possesses P212121 space group, with a = 9.9103(5), b = 13.3597(8), c = 14.5633(8) ?, V = 1928.16(18) ?3, Mr = 402.30, Z = 4, Dc = 1.386 g/cm3, λ = 0.7107 ?, μ(MoKα) = 0.354 mm?1 and F (000) = 840. The structure was refined to R = 0.0280 and wR = 0.0757. In the structure, the pyridine ring adopts a boat conformation.
基金This work was supported by the National Natural Science Foundation of China (No. 20372057 and 20672090)the Foundation of Qinglan Project of Jiangsu Province (No. QL 200512)the Dean Foundation of Xuzhou Education College (No. 2006HX03)
文摘The title compound 5-cyclopropyl-10-（4-fluorophenyl）-7,7-dimethyl-7,8-dihydro- 5H-indeno[1,2-b]quinolne-9,11（6H,10H）-dione was obtained by the reaction of 4-fluorobenzal- dehyde, 2H-indene-1,3-dione and 3-（cyclopropylamino）-5,5-dimethylcyclohex-2-enone in the presence of acetic acid under microwave irradiation. Its structure was confirmed by IR and 1H- NMR spectra. The crystal is of monoclinic, space group P21/c with a = 14.138（3）, b = 8.952（2）, c = 17.140（3）A, β = 102.253（3）°, C27H24FNO2, Mr = 413.47, Z = 4, V = 2119.9（8）A^3, Dc = 1.296 g/cm^3, μ（MoKα） = 0.087 mm^-1, F（000） = 872, the final R = 0.0425 and wR = 0.0905 for 2336 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the pyridine ring adopts a boat conformation and the six-membered ring fused with it assumes a twist boat conformation.
基金This work was supported by the National Natural Science Foundation of China (No. 20372057) the Natural Science Foundation of Jiangsu Province (No. BK2001142)+3 种基金 the Open Foundation of Key Laboratory of Organic Synthesis of Jiangsu Province College of Chemistry and Chemical Engineering Suzhou University (JSK 011) the Key Lab of Biotechnology for Medicinal Plants of Jiangsu Province (01AXL 14)
文摘The title compound (C25H24N4O3) has been prepared by the cyclocondensation of 5-amino-3-methyl-1-phenypyrazol, m-nitrobenaldehyde and dimedone in glycol under microwave irradiation without catalyst. The crystal structure was determined by single-crystal X-ray diffraction to be orthorhombic, space group Pbca with a = 16.3331(10), b = 13.8329(9), c = 19.4163(12) ?, V = 4386.8(5) ?3, Z = 8, Dc = 1.298 g/cm3, μ = 0.087 mm-1, F(000) = 1808, Mr = 428.48, the final R = 0.0519 and wR = 0.1019. X-ray analysis revealed that the pyridine ring is of boat conformation and the six-membered ring fused with it adopts twist boat conformation.② Corresponding author. Tu Shu-Jiang, born in 1957, professor, majoring in the synthesis of organic and heterocycle compounds. E-mail: laotu2001@ 263.net
文摘4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the catalyst.Its structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic crystal system,P-1 space group,a=9.5470(19)?,b=13.637(3)?,c=16.029(3)?,α=75.33(3)°,β=83.62(3)°,γ=70.99(3)°,V=1097.8(7)s assembled into supramolecule structure by intermolecular hydrogen bonds.
文摘Benzoxazinone usually exists in many kinds of plants.It is applied in prepharmacy synthesis,and bioactivity studies,and has been prepared from O-aminophenol and chrol-with alkine and solvent by refluxing for a long time.In this work,2,2’-diphenyl-1,4-benzoxazin-3(4H)-one was solvent-free synthesized under microwave irradiation.The configuration and conformation of the product were determined by 1H NMR,IR,MS,elementary analysis and X-ray crystal analysis.The results of X-ray crystal analysis show that the compound crystallizes in a triclinic system,space group %P%1,cell parameter %a%=0.840 7(1)nm,%b%=0.845 1(1)nm,%c%=2.254 1(3)nm,%α%=96.111(3)°,%β%=97.196(3)°,%γ%=90.229(3)°,%V%= 1^579 6(4)nm3,%Z%=4,%D%c =1.267 Mg/m3,%F%(000)= 632.0,%μ%= 0.08 mm-1.In the compound,oxazinone ring is shown chair conformation,two benzene rings is placed in two sides of oxazinone ring distortedly.In crystal state,a centrosymmetric dimmer is formed %via% hydrogen bonds generated from amides of two near molecules.The benzene rings in a same chemical environment are paralleled by a distance of 0.260 9 nm.It displays aromatic π-π stacking interactions.
