The title compound 2-(2-chloro-4-nitrophenyl)-4-(4-chlorophenyl)-3a,4- diethoxy- 2,3,3a, 4-tetrahydrochromeno[3,4-d][1,2,3]diazaphosphole 2 (C29H30Cl2N3O7P, Mr = 633.44) was synthesized and its structure was cha...The title compound 2-(2-chloro-4-nitrophenyl)-4-(4-chlorophenyl)-3a,4- diethoxy- 2,3,3a, 4-tetrahydrochromeno[3,4-d][1,2,3]diazaphosphole 2 (C29H30Cl2N3O7P, Mr = 633.44) was synthesized and its structure was characterized by IR, MS, ^1H NMR, ^13C NMR, ^31p NMR, elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1^-, a = 9.1549(3), b = 10.7168(4), c = 17.6272(6)A, α = 102.9363(12), β = 90.2713(9), γ = 117.4265(10)°, V= 1484.41(9)A^3, Z= 2,μ(MoKa) = 0.323, F(000) = 658, Z= 2, De= 1.417 g/cm^3, the final R = 0.0687 and wR = 0.2066 for 4943 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the diazaphospholine ring is almost planar and the two ethoxy groups bonded on the 3a- and 4-positions are in trans configurations. Its antiproliferative activity was also tested in vitro against four human tumor cell lines.展开更多
The new title compound 4-chloro-N-(2-(2-nitrophenyl)acetoxy)-N-(m-tolyl)benza- mide (C:2HI7C1N2Os, Mr = 424.82) has been synthesized via the reaction of 4-chloro-N-hydroxy-N- (m-tolyl)benzamide with 2-(2-n...The new title compound 4-chloro-N-(2-(2-nitrophenyl)acetoxy)-N-(m-tolyl)benza- mide (C:2HI7C1N2Os, Mr = 424.82) has been synthesized via the reaction of 4-chloro-N-hydroxy-N- (m-tolyl)benzamide with 2-(2-nitrophenyl)acetyl chloride. The structure of the product was confirmed by 1H NMR, 13C NMR, IR, HRMS (ESI) and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a = 13.0269(10), b =6.7251(6), c = 23.9313(16) A, β = 99.931(6)°, V = 2065.1(3) A3, Z = 4, Dc = 1.366 g/cm3, F(000) = 880,μ = 0.221 mm-1, the final R = 0.0600 and wR = 0.1754 for 1981 observed reflections (I〉 20(/)). X-ray analysis indicates that the chloro-phenyl ring (C(10)℃(15)) and the methyl-substituted benzene ring (C(16)℃(21)) are not coplanar with the nitro-substituted benzene ring (C(1)--C(6)), with the dihedral angle to be 70.78° and 63.72°, respectively. Hydrogen bonds C(2)-H(2)...O(2) and C(7)-H(7B)...O(5) are observed.展开更多
Synthesis of the title compound was carried out by base-catalyzed cyclization of 1-pivaloyl-3-(2-chloro-4-nitrophenyl) thiourea with α-bromoacetone produced in situ. The structure was confirmed by the spectroscopic a...Synthesis of the title compound was carried out by base-catalyzed cyclization of 1-pivaloyl-3-(2-chloro-4-nitrophenyl) thiourea with α-bromoacetone produced in situ. The structure was confirmed by the spectroscopic and elemental analysis and single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1 with unit cell dime sions a = 8.7137(10), b = 10.2010(14), c = 10.6593(13), α = 62.671(9), β = 82.701(10), γ = 79.762(10), V = 827.21(8) ?3, Z = 2.展开更多
文摘The title compound 2-(2-chloro-4-nitrophenyl)-4-(4-chlorophenyl)-3a,4- diethoxy- 2,3,3a, 4-tetrahydrochromeno[3,4-d][1,2,3]diazaphosphole 2 (C29H30Cl2N3O7P, Mr = 633.44) was synthesized and its structure was characterized by IR, MS, ^1H NMR, ^13C NMR, ^31p NMR, elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1^-, a = 9.1549(3), b = 10.7168(4), c = 17.6272(6)A, α = 102.9363(12), β = 90.2713(9), γ = 117.4265(10)°, V= 1484.41(9)A^3, Z= 2,μ(MoKa) = 0.323, F(000) = 658, Z= 2, De= 1.417 g/cm^3, the final R = 0.0687 and wR = 0.2066 for 4943 observed reflections (I 〉 2σ(I)). X-ray analysis reveals that the diazaphospholine ring is almost planar and the two ethoxy groups bonded on the 3a- and 4-positions are in trans configurations. Its antiproliferative activity was also tested in vitro against four human tumor cell lines.
基金Supported by the Fundamental Research Funds for the Central Universities(lzujbky-2010-137)Lanzhou Science and Technology Bureau Program Funds(2012-2-90)
文摘The new title compound 4-chloro-N-(2-(2-nitrophenyl)acetoxy)-N-(m-tolyl)benza- mide (C:2HI7C1N2Os, Mr = 424.82) has been synthesized via the reaction of 4-chloro-N-hydroxy-N- (m-tolyl)benzamide with 2-(2-nitrophenyl)acetyl chloride. The structure of the product was confirmed by 1H NMR, 13C NMR, IR, HRMS (ESI) and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a = 13.0269(10), b =6.7251(6), c = 23.9313(16) A, β = 99.931(6)°, V = 2065.1(3) A3, Z = 4, Dc = 1.366 g/cm3, F(000) = 880,μ = 0.221 mm-1, the final R = 0.0600 and wR = 0.1754 for 1981 observed reflections (I〉 20(/)). X-ray analysis indicates that the chloro-phenyl ring (C(10)℃(15)) and the methyl-substituted benzene ring (C(16)℃(21)) are not coplanar with the nitro-substituted benzene ring (C(1)--C(6)), with the dihedral angle to be 70.78° and 63.72°, respectively. Hydrogen bonds C(2)-H(2)...O(2) and C(7)-H(7B)...O(5) are observed.
文摘Synthesis of the title compound was carried out by base-catalyzed cyclization of 1-pivaloyl-3-(2-chloro-4-nitrophenyl) thiourea with α-bromoacetone produced in situ. The structure was confirmed by the spectroscopic and elemental analysis and single crystal X-ray diffraction data. It crystallizes in the triclinic space group P-1 with unit cell dime sions a = 8.7137(10), b = 10.2010(14), c = 10.6593(13), α = 62.671(9), β = 82.701(10), γ = 79.762(10), V = 827.21(8) ?3, Z = 2.