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
Kinetic resolution of racemic 2-chloro-1-（3,4-dichlorophenyl）ethanol was performed by free Alcaligene sp. lipase-catalyzed irreversible transesterification affording the （R）-isomer with ≥95% ee and the （S）-isom...Kinetic resolution of racemic 2-chloro-1-（3,4-dichlorophenyl）ethanol was performed by free Alcaligene sp. lipase-catalyzed irreversible transesterification affording the （R）-isomer with ≥95% ee and the （S）-isomer with ≥90% ee. The activity of lipase Alcaligene sp. strongly depends on the basicity of the reaction system, and an organic base such as triethylamine can enhance the activity of the lipase and enantioselectivity markedly.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Project supported by the Doctoral Foundation of Qingdao University of Science and Technology （No. 0022266）, the Program for New Century Excellent Talents in Universities （No. NCET-04-0649）, and the Natural Science Foundation of Shandong Province （No. Z2006B01）.
文摘Kinetic resolution of racemic 2-chloro-1-（3,4-dichlorophenyl）ethanol was performed by free Alcaligene sp. lipase-catalyzed irreversible transesterification affording the （R）-isomer with ≥95% ee and the （S）-isomer with ≥90% ee. The activity of lipase Alcaligene sp. strongly depends on the basicity of the reaction system, and an organic base such as triethylamine can enhance the activity of the lipase and enantioselectivity markedly.
