The title compound (+)-(a-hydroxybenzyl)phenylphosphinic acid (C13H13O3P, Mr = 248.20) has been synthesized and characterized by 31P NMR, 1H NMR and elemental analysis. X-ray diffraction analysis at 293(2) K indicates...The title compound (+)-(a-hydroxybenzyl)phenylphosphinic acid (C13H13O3P, Mr = 248.20) has been synthesized and characterized by 31P NMR, 1H NMR and elemental analysis. X-ray diffraction analysis at 293(2) K indicates that the compound belongs to monoclinic system, space group C2 with cell parameters: a = 23.560(8), b = 6.947(2), c = 7.854(3) ? b = 91.273(6)? V = 1285.2(7) 3, Z = 4, Dc = 1.283 g/cm3, F(000) = 520 and m(MoKa) = 0.207 mm-1. The number of independent reflections amounts to 1991, of which 1507 are observed reflections. The crystal structure has been determined by direct methods (SHELXL-97). The structure parameters are refined by full-matrix least-squares on F2 to R = 0.0437 and wR = 0.0893. The flack x parameter is 0.0001. The absolute configuration of the a-carbon in the title compound is S.展开更多
An efficient metal-free strategy for the synthesis of pharmaceutically relevant benzo[α]carbazoles from the derivatives of readily available 2-phenylindole and bio-renewable acetol in an aqueous biphasic system was d...An efficient metal-free strategy for the synthesis of pharmaceutically relevant benzo[α]carbazoles from the derivatives of readily available 2-phenylindole and bio-renewable acetol in an aqueous biphasic system was developed. This protocol employed a sulfone-containing Bronsted acidic ionic liquid as the catalyst, which could be used for five times without a noticeable decrease in its activity and selectivity. Various substituted 2-phenylindoles and α-hydroxyketones participated in the reaction smoothly, with water as the sole byproduct. Mechanistically, the reaction involved the conventional carbon-nucleophile-induced Heyns-type rearrangement and downstream intramolecular olefination.展开更多
The crystal structure of the title compound C_12H_18NO_6P has been determined by X-ray diffraction methods. It belongs to orthorhombic space group Pabc with cell parameters: a=10. 708(5), b=16.151(4), c=17. 615(2) A, ...The crystal structure of the title compound C_12H_18NO_6P has been determined by X-ray diffraction methods. It belongs to orthorhombic space group Pabc with cell parameters: a=10. 708(5), b=16.151(4), c=17. 615(2) A, V=3046. 4 A￣3, Z=8, D_c= 1. 39 g/cm￣3, F(000)=1280, μ=29. 77cm￣(-1) (CuKα), M_r= 303. 25 ,R=0. 065, R_w= 0. 055. In the molecule, the P atom is coordinated by three O and one C atoms with a distorted tetrahedral configuration.展开更多
基金Financial support by the National Natural Science Foundation of China (No.29872016)
文摘The title compound (+)-(a-hydroxybenzyl)phenylphosphinic acid (C13H13O3P, Mr = 248.20) has been synthesized and characterized by 31P NMR, 1H NMR and elemental analysis. X-ray diffraction analysis at 293(2) K indicates that the compound belongs to monoclinic system, space group C2 with cell parameters: a = 23.560(8), b = 6.947(2), c = 7.854(3) ? b = 91.273(6)? V = 1285.2(7) 3, Z = 4, Dc = 1.283 g/cm3, F(000) = 520 and m(MoKa) = 0.207 mm-1. The number of independent reflections amounts to 1991, of which 1507 are observed reflections. The crystal structure has been determined by direct methods (SHELXL-97). The structure parameters are refined by full-matrix least-squares on F2 to R = 0.0437 and wR = 0.0893. The flack x parameter is 0.0001. The absolute configuration of the a-carbon in the title compound is S.
基金supported by the National Natural Science Foundation of China(21761132014,21872060)the Fundamental Research Funds for the Central Universities of China(2016YXZD033)+1 种基金the Fundamental Research Funds for the Central Universities(2019kfyXJJS072)Opening fund of Hubei Key Laboratory of Material Chemistry and Service Failure(2017MCF01K)~~
文摘An efficient metal-free strategy for the synthesis of pharmaceutically relevant benzo[α]carbazoles from the derivatives of readily available 2-phenylindole and bio-renewable acetol in an aqueous biphasic system was developed. This protocol employed a sulfone-containing Bronsted acidic ionic liquid as the catalyst, which could be used for five times without a noticeable decrease in its activity and selectivity. Various substituted 2-phenylindoles and α-hydroxyketones participated in the reaction smoothly, with water as the sole byproduct. Mechanistically, the reaction involved the conventional carbon-nucleophile-induced Heyns-type rearrangement and downstream intramolecular olefination.
文摘The crystal structure of the title compound C_12H_18NO_6P has been determined by X-ray diffraction methods. It belongs to orthorhombic space group Pabc with cell parameters: a=10. 708(5), b=16.151(4), c=17. 615(2) A, V=3046. 4 A￣3, Z=8, D_c= 1. 39 g/cm￣3, F(000)=1280, μ=29. 77cm￣(-1) (CuKα), M_r= 303. 25 ,R=0. 065, R_w= 0. 055. In the molecule, the P atom is coordinated by three O and one C atoms with a distorted tetrahedral configuration.
