A rapid and efficient microwave-assisted synthesis method for the preparation of 3-（lH-benzo[d]imidazol-2-yl）-2-substituted phenyl thiazolidin-4-one （4a, 4b） was described. The structures of 4a and 4b were determi...A rapid and efficient microwave-assisted synthesis method for the preparation of 3-（lH-benzo[d]imidazol-2-yl）-2-substituted phenyl thiazolidin-4-one （4a, 4b） was described. The structures of 4a and 4b were determined by elemental analyses, IR, 1H NMR and X-ray diffraction. In the crystals of compounds 4a and 4b, the imidazole ring and two benzene rings are planar. Interestingly, the dihedral angle between two benzene rings is 71.5° in 4a, while it is almost perpendicular in 4b due to the different benzene substituents. Meanwhile, the thiazolidinone ring is planar in 4a while slightly distorted with an r.m.s deviation of 0.1494（2） A in 4b. The hydrogen bonding interactions observed link the molecules to form a dimeric unit, which may be effective in the stabilization of the structure.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 title compound (C25H17BrClN3) has been synthesized by the reaction of 1-(2- chlorophenyl)-3-(4-bromophenyl)-2-propylene-1-one with 5-amino-3-methyl-1-phenyl pyrazole under microwave irradiation and its structure...The title compound (C25H17BrClN3) has been synthesized by the reaction of 1-(2- chlorophenyl)-3-(4-bromophenyl)-2-propylene-1-one with 5-amino-3-methyl-1-phenyl pyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 9.3798(11), b = 10.6200(13), c = 11.7433(15) ?, α = 72.932(9), β = 78.877(10), γ = 72.045(9)o, V = 1057.0(2) ?3, Z = 2, Dc = 1.492 g/cm3, μ = 2.088 mm -1 , F(000) = 480, Mr = 474.78, the final R = 0.0428 and wR = 0.0879. X-ray analysis revealed that the dihedral angle between the pyrazol and pyridine planes is 6.45o.展开更多
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
The crystal structure of the title compound (C20H20O4, Mr = 324.36) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group Pbcn with a = 15.823(2), b = 18.002(3), c = 11...The crystal structure of the title compound (C20H20O4, Mr = 324.36) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group Pbcn with a = 15.823(2), b = 18.002(3), c = 11.674(2) ?, V = 3325.34(67) ?3, Dc = 1.296 g/cm3, μ = 0.090 mm-1, Z = 8, F(000) = 1376, the final R = 0.0421 and wR = 0.0996. In the molecular structure, the pyran ring is of boat conformation, and the two six-membered rings fused with it adopt twisting-boat conformations.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 und...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）A, V= 1928.16（18）A3 ,Mr = 402.30, Z = 4, Dc= 1.386 g/cm^3, 2 = 0.7107A,μ（MoKα）=0.354mm^-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 (C20H15ClN4O, Mr = 362.81) was synthesized by the reaction of ethyl 2-cyano-3-(2-chlorophenyl)-1-acylate with 5-amino-3-methyl-1-phenylpyrazole under microwave irradiation and its structure was dete...The title compound (C20H15ClN4O, Mr = 362.81) was synthesized by the reaction of ethyl 2-cyano-3-(2-chlorophenyl)-1-acylate with 5-amino-3-methyl-1-phenylpyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 8.8192(19), b = 15.976(3), c = 13.094(3) ? = 103.074(4), V = 1797.1(7) ?, Z = 4, Dc = 1.341 g/cm3, = 0.229 mm-1, F(000) = 752, R = 0.0632 and wR = 0.1278. X-ray analysis reveals that the pyridine ring adopts an envelope conformation. The dihedral angle between the pyrazole and pyridine planes is 2.19, and inter- molecular hydrogen bonds are also observed in the molecule.展开更多
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) A, β = ...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) A, β = 104.77(1)°, V= 3070.4(7) A3, Mr= 303.31, Z = 8, Dc= 1.312 g/cm3, λ = 0.71073 A,μ(MoKα) = 0.098 mm-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,3-acetamido-1-phenyl-4-（2,6-dichloro）benzylidene-5-pyrazolone（C18H13Cl2N3O2,Mr = 374.21）,has been synthesized by one-step condensation of 2,6-dichloroben-zaldehyde with acetic anhydride and 3-am...The title compound,3-acetamido-1-phenyl-4-（2,6-dichloro）benzylidene-5-pyrazolone（C18H13Cl2N3O2,Mr = 374.21）,has been synthesized by one-step condensation of 2,6-dichloroben-zaldehyde with acetic anhydride and 3-amino-1-phenyl-5-pyrazolone under microwave irradiation.The compound was characterized by means of IR and 1H NMR.Its crystal and molecular structure were determined by X-ray diffractometry.It belongs to the orthorhombic system,space group Pbca,with a = 12.5312（13）,b = 8.5495（9）,c = 31.110（3） ,V = 3332.9（6） 3,Z = 8,Dc = 1.492 g/cm3,λ = 0.71073 ,μ（MoKα） = 0.407 mm-1,F（000） = 1536,the final R = 0.0394 and wR = 0.0984.A total of 15894 reflections were collected,of which 3630 were independent（Rint = 0.0362）.There exist three planes in the molecular structure.X-ray analysis reveals that the dihedral angles between planes 1 and 2,1 and 3 and 3 and 2 are 80.89,74.29 and 20.57°,respectively.展开更多
The title compound 2-amino-3-ethoxycarbonyl-4-(4-chlorophenyl)-4H,5H-pyrano- [3,2-c]-benzopyran-5-one (C21H16ClNO5, Mr = 397.80) has been synthesized and characterized by X-ray crystallography. It crystallizes in tric...The title compound 2-amino-3-ethoxycarbonyl-4-(4-chlorophenyl)-4H,5H-pyrano- [3,2-c]-benzopyran-5-one (C21H16ClNO5, Mr = 397.80) has been synthesized and characterized by X-ray crystallography. It crystallizes in triclinic, space group P1 with a = 5.756(1), b = 10.099(1), c = 17.106(3) ? a = 80.49(1), b = 83.13(1), g = 80.07(1), V = 961.8(2) ?, Dc = 1.374 g/cm3, = 0.231 mm-1, Z = 2, F(000) = 412, the final R = 0.0369 and wR = 0.0947. In the molecule the pyran ring is of boat conformation. The intermolecular hydrogen bonds of NH…O(5)(x+2, y+1, z+1) and NH…Cl (x+1, y1, z) as well as intramolecular hydrogen bond NH…O(5) are found.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
The title compound 4-(4-chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydro- pyrimidin-2(H)-one has been synthesized by the reaction of 4-chlorobenzaldehyde, methyl acetoa- cetate and urea using H3BO3 as a catalyst...The title compound 4-(4-chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydro- pyrimidin-2(H)-one has been synthesized by the reaction of 4-chlorobenzaldehyde, methyl acetoa- cetate and urea using H3BO3 as a catalyst under microwave irradiation. Its structure was charac- terized by X-ray single-crystal diffraction techniques with the following data: triclinic, space group P1, a = 5.4513(4), b = 7.619(1), c = 16.118(4) ?, α = 80.42(1), β = 83.43(1), γ = 79.29(1)°, V = 646.19(19) ?3, Mr = 280.70, μ(MoKα) = 0.301 mm-1, Z = 2 and Dc = 1.443 g/cm3. In the molecule the pyrimidine ring is of boat conformation.展开更多
The title compound (C19H29NO4) has been synthesized by the reaction of pro- paldehyde with dimedone and hydroxylamine hydrochloride in glycol under microwave irradiation, and its structure was determined by single-c...The title compound (C19H29NO4) has been synthesized by the reaction of pro- paldehyde with dimedone and hydroxylamine hydrochloride in glycol under microwave irradiation, and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 12.533(1), b = 13.184(2), c = 11.883(2) ?, β = 109.06(1)°, V = 1856.0(5) ?3, Mr = 335.43, Z = 4, Dc = 1.201 g/cm3, λ = 0.71073 ?, μ(MoKα) = 0.083 mm-1 and F(000) = 728. The structure was refined to R = 0.0488 and wR = 0.1456 for 2306 observed reflections with I > 2σ(I). X-ray analysis reveals that the pyridine ring adopts a boat conformation, while two cyclohexanone rings have envelope conformations.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
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
基金Supported by the National High Technology Research and Development (863 Program) of China (No. 2007AA06A402)Key Projects in the National Science and Technology Pillar Program (No. 2006BAC02A15)+1 种基金Key Projects in the National Water Pollution Control and Management Pillar Program(No. 2008ZX07101-003)2011 Key projects of Natural Science of Jiangsu Province-owned Colleges (No. 11KJA610001)
文摘A rapid and efficient microwave-assisted synthesis method for the preparation of 3-（lH-benzo[d]imidazol-2-yl）-2-substituted phenyl thiazolidin-4-one （4a, 4b） was described. The structures of 4a and 4b were determined by elemental analyses, IR, 1H NMR and X-ray diffraction. In the crystals of compounds 4a and 4b, the imidazole ring and two benzene rings are planar. Interestingly, the dihedral angle between two benzene rings is 71.5° in 4a, while it is almost perpendicular in 4b due to the different benzene substituents. Meanwhile, the thiazolidinone ring is planar in 4a while slightly distorted with an r.m.s deviation of 0.1494（2） A in 4b. The hydrogen bonding interactions observed link the molecules to form a dimeric unit, which may be effective in the stabilization of the structure.
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°.
文摘The title compound (C25H17BrClN3) has been synthesized by the reaction of 1-(2- chlorophenyl)-3-(4-bromophenyl)-2-propylene-1-one with 5-amino-3-methyl-1-phenyl pyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 9.3798(11), b = 10.6200(13), c = 11.7433(15) ?, α = 72.932(9), β = 78.877(10), γ = 72.045(9)o, V = 1057.0(2) ?3, Z = 2, Dc = 1.492 g/cm3, μ = 2.088 mm -1 , F(000) = 480, Mr = 474.78, the final R = 0.0428 and wR = 0.0879. X-ray analysis revealed that the dihedral angle between the pyrazol and pyridine planes is 6.45o.
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.
文摘The crystal structure of the title compound (C20H20O4, Mr = 324.36) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group Pbcn with a = 15.823(2), b = 18.002(3), c = 11.674(2) ?, V = 3325.34(67) ?3, Dc = 1.296 g/cm3, μ = 0.090 mm-1, Z = 8, F(000) = 1376, the final R = 0.0421 and wR = 0.0996. In the molecular structure, the pyran ring is of boat conformation, and the two six-membered rings fused with it adopt twisting-boat conformations.
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）A, V= 1928.16（18）A3 ,Mr = 402.30, Z = 4, Dc= 1.386 g/cm^3, 2 = 0.7107A,μ（MoKα）=0.354mm^-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 NNSFC (No. 20372057) the NSF of Jiangsu Province (No. BK2001142)+2 种基金 the Open Foundation of Key Laboratory of Organic Synthesis of Jiangsu Province College of Chemistry and Chemical Engineering Suzhou University (No. S
文摘The title compound (C20H15ClN4O, Mr = 362.81) was synthesized by the reaction of ethyl 2-cyano-3-(2-chlorophenyl)-1-acylate with 5-amino-3-methyl-1-phenylpyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 8.8192(19), b = 15.976(3), c = 13.094(3) ? = 103.074(4), V = 1797.1(7) ?, Z = 4, Dc = 1.341 g/cm3, = 0.229 mm-1, F(000) = 752, R = 0.0632 and wR = 0.1278. X-ray analysis reveals that the pyridine ring adopts an envelope conformation. The dihedral angle between the pyrazole and pyridine planes is 2.19, and inter- molecular hydrogen bonds are also observed in the molecule.
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) A, β = 104.77(1)°, V= 3070.4(7) A3, Mr= 303.31, Z = 8, Dc= 1.312 g/cm3, λ = 0.71073 A,μ(MoKα) = 0.098 mm-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Project supported by the National Natural Science Foundation of China (No. 81071144)Natural Science Foundation of Guangdong Province (No. 06028565 and 9451806001002961)Science and Technology Program of Shenzhen (No. 200727)
文摘The title compound,3-acetamido-1-phenyl-4-（2,6-dichloro）benzylidene-5-pyrazolone（C18H13Cl2N3O2,Mr = 374.21）,has been synthesized by one-step condensation of 2,6-dichloroben-zaldehyde with acetic anhydride and 3-amino-1-phenyl-5-pyrazolone under microwave irradiation.The compound was characterized by means of IR and 1H NMR.Its crystal and molecular structure were determined by X-ray diffractometry.It belongs to the orthorhombic system,space group Pbca,with a = 12.5312（13）,b = 8.5495（9）,c = 31.110（3） ,V = 3332.9（6） 3,Z = 8,Dc = 1.492 g/cm3,λ = 0.71073 ,μ（MoKα） = 0.407 mm-1,F（000） = 1536,the final R = 0.0394 and wR = 0.0984.A total of 15894 reflections were collected,of which 3630 were independent（Rint = 0.0362）.There exist three planes in the molecular structure.X-ray analysis reveals that the dihedral angles between planes 1 and 2,1 and 3 and 3 and 2 are 80.89,74.29 and 20.57°,respectively.
基金Supported by NNSFC (No. 20372057) NSF of Jiangsu Province (No. BK2001142) Jiangsu Education Department (No. 01KJB150008) and the Key Lab of Biotechnology for Medicinal Plants of Jiangsu Province (02AXL 14)
文摘The title compound 2-amino-3-ethoxycarbonyl-4-(4-chlorophenyl)-4H,5H-pyrano- [3,2-c]-benzopyran-5-one (C21H16ClNO5, Mr = 397.80) has been synthesized and characterized by X-ray crystallography. It crystallizes in triclinic, space group P1 with a = 5.756(1), b = 10.099(1), c = 17.106(3) ? a = 80.49(1), b = 83.13(1), g = 80.07(1), V = 961.8(2) ?, Dc = 1.374 g/cm3, = 0.231 mm-1, Z = 2, F(000) = 412, the final R = 0.0369 and wR = 0.0947. In the molecule the pyran ring is of boat conformation. The intermolecular hydrogen bonds of NH…O(5)(x+2, y+1, z+1) and NH…Cl (x+1, y1, z) as well as intramolecular hydrogen bond NH…O(5) are found.
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
基金This work was supported by the NNSFC (No. 20372057) Natural Science Foundation of Jiangsu Province (No. BK2001142)+2 种基金 the Open Foundation of Key Laboratory of Organic Synthesis of Jiangsu Province College of Chemistry and Chemical Engineering Su
文摘The title compound 4-(4-chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydro- pyrimidin-2(H)-one has been synthesized by the reaction of 4-chlorobenzaldehyde, methyl acetoa- cetate and urea using H3BO3 as a catalyst under microwave irradiation. Its structure was charac- terized by X-ray single-crystal diffraction techniques with the following data: triclinic, space group P1, a = 5.4513(4), b = 7.619(1), c = 16.118(4) ?, α = 80.42(1), β = 83.43(1), γ = 79.29(1)°, V = 646.19(19) ?3, Mr = 280.70, μ(MoKα) = 0.301 mm-1, Z = 2 and Dc = 1.443 g/cm3. In the molecule the pyrimidine ring is of boat conformation.
基金This work was supported by the National Natural Science Foundation of China (No. 20372057) the Open Foundation of Key Laboratory of Organic Synthesis of Jiangsu Province+1 种基金 College of Chemistry and Chemical Engineering Suzhou University (No. S8109111) and Key Lab of Biotechnology for Medicinal Plants of Jiangsu Province (No. 01AXL 14)
文摘The title compound (C19H29NO4) has been synthesized by the reaction of pro- paldehyde with dimedone and hydroxylamine hydrochloride in glycol under microwave irradiation, and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 12.533(1), b = 13.184(2), c = 11.883(2) ?, β = 109.06(1)°, V = 1856.0(5) ?3, Mr = 335.43, Z = 4, Dc = 1.201 g/cm3, λ = 0.71073 ?, μ(MoKα) = 0.083 mm-1 and F(000) = 728. The structure was refined to R = 0.0488 and wR = 0.1456 for 2306 observed reflections with I > 2σ(I). X-ray analysis reveals that the pyridine ring adopts a boat conformation, while two cyclohexanone rings have envelope conformations.
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.
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.
