以色酮-吡唑啉酮合成子与3-烯键氧化吲哚为原料,DABCO为催化剂,氯仿为溶剂,于室温发生分子间Michael加成反应后再发生分子内环化反应,合成了14个未见文献报道的吡唑啉酮六氢山酮素骨架拼接氧化吲哚3a^3n,产率75%~89%,dr值7/1~11/1,其结...以色酮-吡唑啉酮合成子与3-烯键氧化吲哚为原料,DABCO为催化剂,氯仿为溶剂,于室温发生分子间Michael加成反应后再发生分子内环化反应,合成了14个未见文献报道的吡唑啉酮六氢山酮素骨架拼接氧化吲哚3a^3n,产率75%~89%,dr值7/1~11/1,其结构经1 H NMR,13 C NMR和HR-MS(ESI-TOF)表征。展开更多
Chlorosulfonyl-containing pyrazolone azo compounds (2a, 2b) have been prepared by reaction of the corresponding sodium sulfonate (1a, 1b) with thionyl chloride in the presence of a catalytic quantity of N,Ndimethylfor...Chlorosulfonyl-containing pyrazolone azo compounds (2a, 2b) have been prepared by reaction of the corresponding sodium sulfonate (1a, 1b) with thionyl chloride in the presence of a catalytic quantity of N,Ndimethylformamide in dry benzene. The effects of reaction temperature, time, catalyst and solvent amount on the yield of 2a and 2b were investigated. The results show that chlorination of 1a and 1b under optimal conditions gives 2a and 2b in 95.5% and 99.2% yield respectively. The given method is facile and suitable for large-scale synthesis.展开更多
The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is g...The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 11.111(2) ? b = 103.92(3)? V = 1341.6(5) 3, Z = 4, Dc = 1.776 g/cm3, Mr = 358.66, F(000) = 716, ?= 2.024 mm1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I > 2(I). The Cu(Ⅱ) ion is six-coordinated by four N atoms of two L ligands and two Cl ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu(Ⅱ) ions, resulting in an infinite chain structure.展开更多
A series of novel pyrazoles compounds were synthesized by the reaction of five kinds of substitute α-bromoacetophenone with pyrazole intermediates which was prepared by the reaction of chalcones and thiosemicarbazone...A series of novel pyrazoles compounds were synthesized by the reaction of five kinds of substitute α-bromoacetophenone with pyrazole intermediates which was prepared by the reaction of chalcones and thiosemicarbazones. This method has some advantages such as mild reaction condition, easy operation and higher yield. All the compounds were confirmed by elemental analysis, IR and 1H NMR.展开更多
The title compound, C16H14N4S, has been synthesized by the reaction of pentane-2,4-dione with 5-amino-3-benzylthio-4-cyano-1-H-pyrazole in ethanol, and its crystal structure was determined by X-ray diffraction method....The title compound, C16H14N4S, has been synthesized by the reaction of pentane-2,4-dione with 5-amino-3-benzylthio-4-cyano-1-H-pyrazole in ethanol, and its crystal structure was determined by X-ray diffraction method. The crystal is of monoclinic, space group P21/n with a = 8.699(3), b = 23.139(9), c = 7.536(3) ? b = 92.400(8), V = 1515.5(10) 3, Z = 4, Mr = 294037, Dc = 1.290 g/cm3, = 0.71073 ? (MoKa) = 0.212 mm-1 and F(000) = 616. The structure was refined to R = 0.0533 and wR = 0.1141 for 2672 unique reflections with Rint = 0.06. The structure is a dimmer linked by intermolecular contact S(1)…HC(8) with the S(1)C(8) distance of 3.875 and the angle of 164.8.展开更多
A series of N-dioctylmethyl-2,7-carbazole-alt-5,7-bis（thiophen-2-yl）-2,3-biphenylthieno[3,4-b]pyrazine （PCz-3ThPz-Ph） co- polymeric derivatives appending various donor units in two phenyl rings, namely, PCz-3ThPz-...A series of N-dioctylmethyl-2,7-carbazole-alt-5,7-bis（thiophen-2-yl）-2,3-biphenylthieno[3,4-b]pyrazine （PCz-3ThPz-Ph） co- polymeric derivatives appending various donor units in two phenyl rings, namely, PCz-3ThPz-PhTh, PCz-3ThPz-PhF1, PCz-3ThPz-PhCz, and PCz-3ThPz-PhTpa were synthesized and characterized. The effect of these appending donor units, e.g., thiophene （Th）, fluorene （F1）, carbazole （Cz）, and triarylamine （Tpa）, was investigated on dispersible, optical, electrochemical, and photovoltaic properties for their polymers. The copolymers of PCz-3ThPz-PhCz and PCz-3ThPz-PhTpa containing Cz or Tpa units exhibited higher short-circuit current density （Jsc） and power conversion efficiency （PCE） in their bulk heterojunction polymeric solar cells. The highest PCE of 1.66% and Jsc of 7.16 mA cm-2 were obtained in a device with the PCz-3ThPz-PhCz/PC61BM blend under AM 1.5 G irradiation （100 mW cm 2）; these values are 1.78 and 1.59 times higher than the corresponding values for the PCz-3ThPz-Ph-based device. When PC61BM was placed by PC71BM, the PCz-3ThPz-PhCz-based device displayed an enhanced PCE of 2.98% and a Jsc of 10.88 mA cm-2. This work demonstrated that appending additional hole-transporting units of Cz and Tpa into the side-chain of a polymer with a D-A backbone can significantly enhance the photovoltaic performance of their resultant polymers.展开更多
文摘以色酮-吡唑啉酮合成子与3-烯键氧化吲哚为原料,DABCO为催化剂,氯仿为溶剂,于室温发生分子间Michael加成反应后再发生分子内环化反应,合成了14个未见文献报道的吡唑啉酮六氢山酮素骨架拼接氧化吲哚3a^3n,产率75%~89%,dr值7/1~11/1,其结构经1 H NMR,13 C NMR和HR-MS(ESI-TOF)表征。
基金Project supported by the National Natural Science Foundation of China (No. 21572047)the Plan for Scientific Innovation Talents of Henan Province (No. 184200510012)~~
文摘Chlorosulfonyl-containing pyrazolone azo compounds (2a, 2b) have been prepared by reaction of the corresponding sodium sulfonate (1a, 1b) with thionyl chloride in the presence of a catalytic quantity of N,Ndimethylformamide in dry benzene. The effects of reaction temperature, time, catalyst and solvent amount on the yield of 2a and 2b were investigated. The results show that chlorination of 1a and 1b under optimal conditions gives 2a and 2b in 95.5% and 99.2% yield respectively. The given method is facile and suitable for large-scale synthesis.
基金This work was supported by the National Natural Science Foundation of China (No.20001007 20131020) Natural Science Foundation of the Chinese Academy of Sciences (KJCX2-H3) and Fujian province (2000F006)
文摘The title complex, [Cu(L)Cl2]n (L = 2,5-di-2-pyridyl-1,3,4-oxodiazole) 1, has been obtained from the reaction of 3,6-di-2-pyridyl-1,2,4,5-tetrazine (bptz) and CuCl2?H2O in a mixture solvent of CH3CN and CH2Cl2 (L is generated from the metal-assisted hydrolysis reaction of bptz) and structurally characterized. It crystallizes in space group C2/c of monoclinic system with cell parameters: a = 9.812(2), b = 12.679(3), c = 11.111(2) ? b = 103.92(3)? V = 1341.6(5) 3, Z = 4, Dc = 1.776 g/cm3, Mr = 358.66, F(000) = 716, ?= 2.024 mm1 and S = 1.004. The final R = 0.0346 and wR = 0.0938 for 1011 observed reflections with I > 2(I). The Cu(Ⅱ) ion is six-coordinated by four N atoms of two L ligands and two Cl ions in a distorted octahedral geometry. The ligand L acts as a bis-bidentate ligand to bridge the Cu(Ⅱ) ions, resulting in an infinite chain structure.
基金The authors are extremely grateful to the National Nature Science Foundation of China for supporting this research （No.20962018, No20862015, No.20762009 and No.20562011）.
文摘A series of novel pyrazoles compounds were synthesized by the reaction of five kinds of substitute α-bromoacetophenone with pyrazole intermediates which was prepared by the reaction of chalcones and thiosemicarbazones. This method has some advantages such as mild reaction condition, easy operation and higher yield. All the compounds were confirmed by elemental analysis, IR and 1H NMR.
基金The project was supported by the National Natural Science Foundation of China (No. 20172031) and the Research Fund for the Doctoral Program of Ministry of Education China
文摘The title compound, C16H14N4S, has been synthesized by the reaction of pentane-2,4-dione with 5-amino-3-benzylthio-4-cyano-1-H-pyrazole in ethanol, and its crystal structure was determined by X-ray diffraction method. The crystal is of monoclinic, space group P21/n with a = 8.699(3), b = 23.139(9), c = 7.536(3) ? b = 92.400(8), V = 1515.5(10) 3, Z = 4, Mr = 294037, Dc = 1.290 g/cm3, = 0.71073 ? (MoKa) = 0.212 mm-1 and F(000) = 616. The structure was refined to R = 0.0533 and wR = 0.1141 for 2672 unique reflections with Rint = 0.06. The structure is a dimmer linked by intermolecular contact S(1)…HC(8) with the S(1)C(8) distance of 3.875 and the angle of 164.8.
基金supported by the major program for cultivation of the National Natural Science Foundation of China(91233112)the National Natural Science Foundation of China(21172187,50973093,51403178)+3 种基金the Innovation Group and Xiangtan Joint Project of the Hunan Natural Science Foundation(12JJ7002,12JJ8001)the Scientific Research Fund of Hunan Provincial Education Department(11CY023,12B123)the Open Fund of the State Key Laboratory of Luminescent Materials and Devices(South China University of Technology,No.2014-skllmd-10)the Postgraduate Science Foundation for Innovation in Hunan Province(CX2014B257,CX2011B263)
文摘A series of N-dioctylmethyl-2,7-carbazole-alt-5,7-bis（thiophen-2-yl）-2,3-biphenylthieno[3,4-b]pyrazine （PCz-3ThPz-Ph） co- polymeric derivatives appending various donor units in two phenyl rings, namely, PCz-3ThPz-PhTh, PCz-3ThPz-PhF1, PCz-3ThPz-PhCz, and PCz-3ThPz-PhTpa were synthesized and characterized. The effect of these appending donor units, e.g., thiophene （Th）, fluorene （F1）, carbazole （Cz）, and triarylamine （Tpa）, was investigated on dispersible, optical, electrochemical, and photovoltaic properties for their polymers. The copolymers of PCz-3ThPz-PhCz and PCz-3ThPz-PhTpa containing Cz or Tpa units exhibited higher short-circuit current density （Jsc） and power conversion efficiency （PCE） in their bulk heterojunction polymeric solar cells. The highest PCE of 1.66% and Jsc of 7.16 mA cm-2 were obtained in a device with the PCz-3ThPz-PhCz/PC61BM blend under AM 1.5 G irradiation （100 mW cm 2）; these values are 1.78 and 1.59 times higher than the corresponding values for the PCz-3ThPz-Ph-based device. When PC61BM was placed by PC71BM, the PCz-3ThPz-PhCz-based device displayed an enhanced PCE of 2.98% and a Jsc of 10.88 mA cm-2. This work demonstrated that appending additional hole-transporting units of Cz and Tpa into the side-chain of a polymer with a D-A backbone can significantly enhance the photovoltaic performance of their resultant polymers.
