Aim To investigate the alkylation of 2-thiopyrimidine. Methods Treating the starting material 2-thiopyrimidine with chloromethyl ethers via a procedure of K2CO3 in DMF or with alkyl halide in CH3ONa-CH3OH at room temp...Aim To investigate the alkylation of 2-thiopyrimidine. Methods Treating the starting material 2-thiopyrimidine with chloromethyl ethers via a procedure of K2CO3 in DMF or with alkyl halide in CH3ONa-CH3OH at room temperature, to obtain the corresponding regioselective 2-S-allkyl pyrimidines. The products were determined by JH NMR, 2D NMR, IR and MS spectra. Results 2-S-alkyl-pyrimidines were regioselectively synthesized. Conclusion In different conditions with different alkyl halides, 2- thiouracil could be converted into the corresponding 2-S-alkylpyrimidines regioselectively.展开更多
The title complex [Cu(NO3)2(H2O)2(3,3-azpy)2] (3,3?azpy = 3,3?azobispyridine) has been synthesized and characterized, and its crystal belongs to the triclinic system, space group P with the following crystallographic ...The title complex [Cu(NO3)2(H2O)2(3,3-azpy)2] (3,3?azpy = 3,3?azobispyridine) has been synthesized and characterized, and its crystal belongs to the triclinic system, space group P with the following crystallographic parameters: a = 7.4161(2), b = 8.1754(3), c = 10.7545(4) ? a = 92.958(2), b = 109.978(1), g = 93.369(2)? V = 609.96(4) ?, C20H20N10CuO8, Mr = 592.00, Dc = 1.612 g/cm3, m(MoKa) = 0.964 mm-1, F(000) = 303, Z = 1, the final R = 0.0494 and wR = 0.1269 for 1945 observed reflections (I > 2s(I)). X-ray analysis reveals that the Cu atom adopts a distorted octahedral (4 + 2) coordination. The four closer donor atoms include two N atoms of 3,3?azpy and two O atoms of the coordination aqua with the CuN and CuO distances of 2.014(3) and 1.974(3) ? respectively. Two longer out-of-plane CuO bonds (2.450(3) ? from nitrate complete the strongly distorted octahedral coordination of the Cu atom. Hydrogen bonds are formed through H atoms of each coordination aqua with the remaining N atoms of 3,3?azpy and O atoms of nitrate. A two-dimensional network is constructed by hydrogen bonds and p-p interactions.展开更多
The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group C2/c with a = 18.520(2), b = 7.8910(1), c = 21.728(3) A, β = ...The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group C2/c with a = 18.520(2), b = 7.8910(1), c = 21.728(3) A, β = 104.77(1)°, V= 3070.4(7) A3, Mr= 303.31, Z = 8, Dc= 1.312 g/cm3, λ = 0.71073 A,μ(MoKα) = 0.098 mm-1 and F(000) = 1280. The structure was refined to R = 0.0486 and wR = 0.1287. There exist intermolecular hydrogen bonds in the crystal.展开更多
Time-dependent density functional theory （TDDFT） and femtosecond transient absorption spectroscopy were used to investigate the photophysical properties of 2,3-dihydro-3-keto-lH- pyrido[3,2,1-kl]phenothiazine （PTZ4...Time-dependent density functional theory （TDDFT） and femtosecond transient absorption spectroscopy were used to investigate the photophysical properties of 2,3-dihydro-3-keto-lH- pyrido[3,2,1-kl]phenothiazine （PTZ4） and 3-keto-lH-pyrido[3,2,1-kl]phenothiazine （PTZ5）. The calculated results obtained from TDDFT suggest that the red-shifts of the absorption spectra of these two fluorophores in methanol are due to the formation of hydrogen-bonded complexes at the ground state. Four conformers of PTZ4 were obtained by TDDFT. The two fluorescence peaks of PTZ4 in tetrahydrofuran （THF） came from the ICT states of the four conformers. The fluorescence of PTZ4 in THF showed a dependence on the excitation wavelength because of butterfly bending. The excited state dynamics of PTZ4 in THF and methanol were obtained by transient absorption spectroscopy. The lifetime of the excited PTZ4 in methanol was 53.8 ps, and its relaxation from the LE state to the ICT state was completed within several picoseconds. The short lifetime of excited PTZ4 in methanol was due to the formation of out-of-plane model hydrogen bonds between PTZ4 and methanol at the excited state.展开更多
基金National Nature Science Foundation of China(NO.20172007).
文摘Aim To investigate the alkylation of 2-thiopyrimidine. Methods Treating the starting material 2-thiopyrimidine with chloromethyl ethers via a procedure of K2CO3 in DMF or with alkyl halide in CH3ONa-CH3OH at room temperature, to obtain the corresponding regioselective 2-S-allkyl pyrimidines. The products were determined by JH NMR, 2D NMR, IR and MS spectra. Results 2-S-alkyl-pyrimidines were regioselectively synthesized. Conclusion In different conditions with different alkyl halides, 2- thiouracil could be converted into the corresponding 2-S-alkylpyrimidines regioselectively.
基金the funds of the Key Laboratory of Organic Syntheses of Jiansu province, and the funds of the State Key Laboratory of Structural Chemistry
文摘The title complex [Cu(NO3)2(H2O)2(3,3-azpy)2] (3,3?azpy = 3,3?azobispyridine) has been synthesized and characterized, and its crystal belongs to the triclinic system, space group P with the following crystallographic parameters: a = 7.4161(2), b = 8.1754(3), c = 10.7545(4) ? a = 92.958(2), b = 109.978(1), g = 93.369(2)? V = 609.96(4) ?, C20H20N10CuO8, Mr = 592.00, Dc = 1.612 g/cm3, m(MoKa) = 0.964 mm-1, F(000) = 303, Z = 1, the final R = 0.0494 and wR = 0.1269 for 1945 observed reflections (I > 2s(I)). X-ray analysis reveals that the Cu atom adopts a distorted octahedral (4 + 2) coordination. The four closer donor atoms include two N atoms of 3,3?azpy and two O atoms of the coordination aqua with the CuN and CuO distances of 2.014(3) and 1.974(3) ? respectively. Two longer out-of-plane CuO bonds (2.450(3) ? from nitrate complete the strongly distorted octahedral coordination of the Cu atom. Hydrogen bonds are formed through H atoms of each coordination aqua with the remaining N atoms of 3,3?azpy and O atoms of nitrate. A two-dimensional network is constructed by hydrogen bonds and p-p interactions.
基金Supported by the Natural Science Foundation of Jiangsu province(No.BK2001142)the Natural Science Foundation of Jiangsu Education Department(No.01KJB150008)
文摘The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group C2/c with a = 18.520(2), b = 7.8910(1), c = 21.728(3) A, β = 104.77(1)°, V= 3070.4(7) A3, Mr= 303.31, Z = 8, Dc= 1.312 g/cm3, λ = 0.71073 A,μ(MoKα) = 0.098 mm-1 and F(000) = 1280. The structure was refined to R = 0.0486 and wR = 0.1287. There exist intermolecular hydrogen bonds in the crystal.
文摘Time-dependent density functional theory （TDDFT） and femtosecond transient absorption spectroscopy were used to investigate the photophysical properties of 2,3-dihydro-3-keto-lH- pyrido[3,2,1-kl]phenothiazine （PTZ4） and 3-keto-lH-pyrido[3,2,1-kl]phenothiazine （PTZ5）. The calculated results obtained from TDDFT suggest that the red-shifts of the absorption spectra of these two fluorophores in methanol are due to the formation of hydrogen-bonded complexes at the ground state. Four conformers of PTZ4 were obtained by TDDFT. The two fluorescence peaks of PTZ4 in tetrahydrofuran （THF） came from the ICT states of the four conformers. The fluorescence of PTZ4 in THF showed a dependence on the excitation wavelength because of butterfly bending. The excited state dynamics of PTZ4 in THF and methanol were obtained by transient absorption spectroscopy. The lifetime of the excited PTZ4 in methanol was 53.8 ps, and its relaxation from the LE state to the ICT state was completed within several picoseconds. The short lifetime of excited PTZ4 in methanol was due to the formation of out-of-plane model hydrogen bonds between PTZ4 and methanol at the excited state.
