The crystal structure of the title compound ethyl 3-（4-chlorophenyl）-3,4-dihydro-6- methyl-4-oxo-2-（pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate （C20H20ClN3O4, Mr= 401.84） has been prepared and determined...The crystal structure of the title compound ethyl 3-（4-chlorophenyl）-3,4-dihydro-6- methyl-4-oxo-2-（pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate （C20H20ClN3O4, Mr= 401.84） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215（9）, b = 8.5311（4）, c = 21.6886（9） A^°, β = 91.607（1）°, V = 3814.0（3）A^°^3, Z = 8, Dc = 1.400 g/cm^3, F（000） = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.展开更多
The esterifications of 9-（hydroxyimino）-4-methyl-8,9-dihydrofuro[2,3-h]chromen-2-one （4） with acid chlorides afforded normal oxime-esters 3a-e in 35-78% yields in presence of excessive 4-dimethylaminopyridine as t...The esterifications of 9-（hydroxyimino）-4-methyl-8,9-dihydrofuro[2,3-h]chromen-2-one （4） with acid chlorides afforded normal oxime-esters 3a-e in 35-78% yields in presence of excessive 4-dimethylaminopyridine as the acid scavenger, whereas the reactions gave unexpected 8-substituted products N-（8-chloro-4-methyl-2-oxo-2H-furo-[2,3-h]chromen-9-yl）amides （5a-c） and 4-methyl-2,9-dioxo-8,9-dihydro-2H-furo[2,3-h]chromen-8-ylcarboxyloates （6d-e） by using excessive acid chlorides. The structures of 10 new compounds were determined by 1H NMR, 13C NMR, MS and HRMS, and the possible mechanism for the formation of unexpected products 5a--c and 6d-e was also proposed.展开更多
A metal-organic coordination polymer, [Cd（C15H10N4）（C6H8O4）]2n （1, C15H10N4： 2-methyl-pyrazino-[2,3-f][1,10]-phenanthroline （mpphen）, C6H8O4： adipate）, was synthesized via hydrothermal synthesis. The polymer...A metal-organic coordination polymer, [Cd（C15H10N4）（C6H8O4）]2n （1, C15H10N4： 2-methyl-pyrazino-[2,3-f][1,10]-phenanthroline （mpphen）, C6H8O4： adipate）, was synthesized via hydrothermal synthesis. The polymer was characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. X-ray diffraction shows that 1 is a cadmium polymer constructed by adipate-bridged dmuclear clusters, and each adipate connects two clusters to form a two-dimen- sional planar structure. Crystal data for 1： monoclinic, space group C2/c, a = 22.403（9）, b = 16.039（6）, c = 13.808（6） A, β= 125.262（6）°, V = 4051（3） A3, Mr = 502.79, Dc = 1.649 g/eraa, μ（MoKa） = 1.114 mm^-1, F（000） = 2016, Z = 8, the final R = 0.0509 and wR = 0.1054 for 1509 observed reflections （I 〉 2σ（I））.展开更多
The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been conf...The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been confirmed by IR, 1H NMR, 13C NMR, LC-MS （ESI） and single-crystal X-ray diffraction. （R）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate crystallizes in monoclinic, space group P21/c with a = 11.867（2）, b = 8.4087（2）, c = 14.325（6） A^°, β = 117.59（2）°, Z = 4, V = 1266.9（6） A^°3, Dc = 1.307 g/cm^3, F（000） = 528, μ（MoKα） = 0.097 mm-1, R = 0.0453 and wR = 0.1237; （S）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate belongs to the triclinic system, space group P with a = 8.2647（17）, b = 8.7034（17）, c = 9.5479（19） A^°, α = 105.33（3）, β = 100.95（3）, γ = 105.14（3）°, Z = 2, V = 614.1（2） A^°3, Dc = 1.348 g/cm^3, F（000） = 264, μ（MoKα） = 0.10 mm-1, R = 0.0613 and wR = 0.1037. Both of the molecules prefer to form crystal packing through C–H…O hydrogen bonds.展开更多
基金supported by the Natural Science Foundation of Hubei Province (2006ABB016)Key Science Research Project of Hubei Provincial Department of Education (No.D200724001) the Science Research Project of Yunyang Medical College (No. 2006QDJ16)
文摘The crystal structure of the title compound ethyl 3-（4-chlorophenyl）-3,4-dihydro-6- methyl-4-oxo-2-（pyrrolidin-1-yl）furo[2,3-d]pyrimidine-5-carboxylate （C20H20ClN3O4, Mr= 401.84） has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 20.6215（9）, b = 8.5311（4）, c = 21.6886（9） A^°, β = 91.607（1）°, V = 3814.0（3）A^°^3, Z = 8, Dc = 1.400 g/cm^3, F（000） = 1680, μ = 0.233 mm^-1, R = 0.0718 and wR = 0.1545 for 6717 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals two crystallographically independent molecules in the asymmetric unit.
基金grants from the National Natural Science Foundation of China (No.20272010 and 20672022)
文摘The esterifications of 9-（hydroxyimino）-4-methyl-8,9-dihydrofuro[2,3-h]chromen-2-one （4） with acid chlorides afforded normal oxime-esters 3a-e in 35-78% yields in presence of excessive 4-dimethylaminopyridine as the acid scavenger, whereas the reactions gave unexpected 8-substituted products N-（8-chloro-4-methyl-2-oxo-2H-furo-[2,3-h]chromen-9-yl）amides （5a-c） and 4-methyl-2,9-dioxo-8,9-dihydro-2H-furo[2,3-h]chromen-8-ylcarboxyloates （6d-e） by using excessive acid chlorides. The structures of 10 new compounds were determined by 1H NMR, 13C NMR, MS and HRMS, and the possible mechanism for the formation of unexpected products 5a--c and 6d-e was also proposed.
文摘A metal-organic coordination polymer, [Cd（C15H10N4）（C6H8O4）]2n （1, C15H10N4： 2-methyl-pyrazino-[2,3-f][1,10]-phenanthroline （mpphen）, C6H8O4： adipate）, was synthesized via hydrothermal synthesis. The polymer was characterized by elemental analysis, IR, TG and single-crystal X-ray diffraction. X-ray diffraction shows that 1 is a cadmium polymer constructed by adipate-bridged dmuclear clusters, and each adipate connects two clusters to form a two-dimen- sional planar structure. Crystal data for 1： monoclinic, space group C2/c, a = 22.403（9）, b = 16.039（6）, c = 13.808（6） A, β= 125.262（6）°, V = 4051（3） A3, Mr = 502.79, Dc = 1.649 g/eraa, μ（MoKa） = 1.114 mm^-1, F（000） = 2016, Z = 8, the final R = 0.0509 and wR = 0.1054 for 1509 observed reflections （I 〉 2σ（I））.
基金supported by the National Natural Science Foundation of China(No.31572042)Natural Science Foundation of Heilongjiang Province(B201303)the Research Science Foundation in Technology Innovation of Harbin(No.2015RAYXJ010)
文摘The new title compound, chiral 2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）- 2-oxoethyl acetate, has been synthesized via reduction, cyclization and acylation reaction. The structure of the product has been confirmed by IR, 1H NMR, 13C NMR, LC-MS （ESI） and single-crystal X-ray diffraction. （R）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate crystallizes in monoclinic, space group P21/c with a = 11.867（2）, b = 8.4087（2）, c = 14.325（6） A^°, β = 117.59（2）°, Z = 4, V = 1266.9（6） A^°3, Dc = 1.307 g/cm^3, F（000） = 528, μ（MoKα） = 0.097 mm-1, R = 0.0453 and wR = 0.1237; （S）-2-（3-methyl-2,3-dihydrobenzo[b][1,4]oxazin-4-yl）-2-oxoethyl acetate belongs to the triclinic system, space group P with a = 8.2647（17）, b = 8.7034（17）, c = 9.5479（19） A^°, α = 105.33（3）, β = 100.95（3）, γ = 105.14（3）°, Z = 2, V = 614.1（2） A^°3, Dc = 1.348 g/cm^3, F（000） = 264, μ（MoKα） = 0.10 mm-1, R = 0.0613 and wR = 0.1037. Both of the molecules prefer to form crystal packing through C–H…O hydrogen bonds.
