The crystal structure of 7α-[（R）-1-hydroxyl-1-methyl-3-（thien-2-yl）propyl]-6,14-endoethanotetrahydrothebaine （C29H37NO4S, Mr=495.66） has been determined by single-crystal X-ray diffraction analysis. The crystal...The crystal structure of 7α-[（R）-1-hydroxyl-1-methyl-3-（thien-2-yl）propyl]-6,14-endoethanotetrahydrothebaine （C29H37NO4S, Mr=495.66） has been determined by single-crystal X-ray diffraction analysis. The crystal belongs orthorhombic, space group P212121 with α=10.063（4）, b=12.571（5）, c=19.626（8）A°, V=2482.9（17）A°^3, Z=4, Dc=1.326 g/cm^3,μ=0.167 mm^-1, F（000）=1064, the final R=0.0537 and wR=0.0888. The C（7） substituent is l-hy-droxyl-1-methyl-3-（thienyl-2-）propyl group adopting R-configuration. The N-methyl group is located at the equatorial position as expected. The crystal structure shows the presence of intra- molecular hydrogen bonds, O（1）-H（1）…O（2）.展开更多
The intermediate of d-biotin, (3aS,6aR)-1,3-dibenzyltetrahydro-1H-thieno[3,4- d]-imidazole-2(3H)-one-4-ylidenepentanoil acid was synthesized from (3aS,6aR)-1,3-dibenzylte- trahyro-4H-thieno[3,4-d]-imidazole-2,4(1H)-di...The intermediate of d-biotin, (3aS,6aR)-1,3-dibenzyltetrahydro-1H-thieno[3,4- d]-imidazole-2(3H)-one-4-ylidenepentanoil acid was synthesized from (3aS,6aR)-1,3-dibenzylte- trahyro-4H-thieno[3,4-d]-imidazole-2,4(1H)-dione by using the Grignard reaction. The structure of 3 was characterized by IR, 1H NMR and MS, and the absolute configuration was further confirmed by X-ray crystal structure analysis. Compound 3 crystallizes in monoclinic, space group P21 with a = 11.030(2), b = 7.783(2), c = 12.797(2) , b = 93.44(1)o, Z = 2, Mr = 422.53 (C24H26N2O3S), V = 1096.3(6) 3, = 0.177 mm-1, Dc = 1.280 g/cm3, F(000) = 448 and T = 293(2) K. The final R = 0.0737 and Rw = 0.1974 for 1009 observed reflections with I >2s(I).展开更多
基金The project was supported by the NNSFC (No. 30271492)
文摘The crystal structure of 7α-[（R）-1-hydroxyl-1-methyl-3-（thien-2-yl）propyl]-6,14-endoethanotetrahydrothebaine （C29H37NO4S, Mr=495.66） has been determined by single-crystal X-ray diffraction analysis. The crystal belongs orthorhombic, space group P212121 with α=10.063（4）, b=12.571（5）, c=19.626（8）A°, V=2482.9（17）A°^3, Z=4, Dc=1.326 g/cm^3,μ=0.167 mm^-1, F（000）=1064, the final R=0.0537 and wR=0.0888. The C（7） substituent is l-hy-droxyl-1-methyl-3-（thienyl-2-）propyl group adopting R-configuration. The N-methyl group is located at the equatorial position as expected. The crystal structure shows the presence of intra- molecular hydrogen bonds, O（1）-H（1）…O（2）.
基金a Grant-in-Aid (96107) for Scientific Research from the Ministry of Chemical Industry of China
文摘The intermediate of d-biotin, (3aS,6aR)-1,3-dibenzyltetrahydro-1H-thieno[3,4- d]-imidazole-2(3H)-one-4-ylidenepentanoil acid was synthesized from (3aS,6aR)-1,3-dibenzylte- trahyro-4H-thieno[3,4-d]-imidazole-2,4(1H)-dione by using the Grignard reaction. The structure of 3 was characterized by IR, 1H NMR and MS, and the absolute configuration was further confirmed by X-ray crystal structure analysis. Compound 3 crystallizes in monoclinic, space group P21 with a = 11.030(2), b = 7.783(2), c = 12.797(2) , b = 93.44(1)o, Z = 2, Mr = 422.53 (C24H26N2O3S), V = 1096.3(6) 3, = 0.177 mm-1, Dc = 1.280 g/cm3, F(000) = 448 and T = 293(2) K. The final R = 0.0737 and Rw = 0.1974 for 1009 observed reflections with I >2s(I).
