Ga（ClO4）3-catalyzed reaction of 1,2-aryldiamines and α-bromoketones to afford 2-substituted quinoxalines in good yields is described.The reaction proceeded via grinding process with 10%（molar fraction） catalyst u...Ga（ClO4）3-catalyzed reaction of 1,2-aryldiamines and α-bromoketones to afford 2-substituted quinoxalines in good yields is described.The reaction proceeded via grinding process with 10%（molar fraction） catalyst under solvent-free conditions at room temperature.For unsymmetrical o-phenylenediamines bearing electron-withdrawing groups,regio-selective quinoxalines were obtained.展开更多
A novel technique to extend template application ofanodic porous alumina to Si has been reported.First,porous alumina template about 400 nm thick was prepared on silicon substrate by anodizing thin aluminum film with ...A novel technique to extend template application ofanodic porous alumina to Si has been reported.First,porous alumina template about 400 nm thick was prepared on silicon substrate by anodizing thin aluminum film with high purity of 99.99%in 15 wt.%sulfuric acid under a constant voltage of 20 V and at an electrolyte temperature of 5°C.Then,amorphous Si layer approximately 50nm in thickness was deposited onto the surface of template by using electron beam evaporation technique followed by an Xe ion beam bombardment,upon which as-coated Si layer at the pore mouth could be removed into pores smootlly.Three runs were performed by repeating above process of deposition and post bombardment.Finally,samples were annealed at 800°C for 30min in nitrogen.Transmission electron microscopy and x-ray diffraction analysis reveal Si nanocrystals with a size of 15-20nm being formed in the pores of template.展开更多
The title compound 1,5-diphenyl-3-phenacylthio-1H-1,2,4-triazole 2 （C22H17- N3OS, Mr = 371.45） was prepared by the reaction of 1-benzoyl-3-phenyl-aminothiourea 1 with 2-bromoacetophenone. The crystal is of triclinic...The title compound 1,5-diphenyl-3-phenacylthio-1H-1,2,4-triazole 2 （C22H17- N3OS, Mr = 371.45） was prepared by the reaction of 1-benzoyl-3-phenyl-aminothiourea 1 with 2-bromoacetophenone. The crystal is of triclinic, space group P^1-, a = 8.906（3）, b = 9.853（3）, c = 11.226（4）A, α= 100.562（5）, β= 101.285（5）, γ. = 105.096（6）^c, Z = 2, V = 903.7（5） ]A^3, Dc= 1.365 g/cm^3,μ（MoKa） = 0.196 mm^-1, F（000） = 388, the final R = 0.0506 and wR = 0.0985 for 2532 observed reflections （I〉 2σ（I））. Its formation mechanism was proposed.展开更多
,3-Disubstituted quinoxalines were synthesized from α-acetylthioformanilide and ophenylenediamine. Further studies sliowed that there existed competitive re- actions. One was a condensation reaction which produced su...,3-Disubstituted quinoxalines were synthesized from α-acetylthioformanilide and ophenylenediamine. Further studies sliowed that there existed competitive re- actions. One was a condensation reaction which produced substituted quinoxaline and the other was a substitution reaction which produced substituted quinoxaline-2- thione.展开更多
The title compound 2, 3-diethoxycarbonyl-4-phenyl-5-morpholinylthiophene (C20H23NO5S, Mr=389. 47) was obtained by the reaction of a-thiobenzoylth-ioformmorpholine with diethyl acetylene dicarboxylate - The crystal is ...The title compound 2, 3-diethoxycarbonyl-4-phenyl-5-morpholinylthiophene (C20H23NO5S, Mr=389. 47) was obtained by the reaction of a-thiobenzoylth-ioformmorpholine with diethyl acetylene dicarboxylate - The crystal is prismatic, spacegroup P1 ( 2), with unit cell constants 2337 observed reflections . X-ray analysis reveals that interatomic dis-tances for C(1 ) -C(2) and C(3) -C (4) are 1. 393 (4), 1. 370 (4) , respectively,which show that they are C=C double bond. The atoms of C(1 ), C(2), C(3), C(4)and S form a thiophene ring. The dihedral ang1es between thiophene ring and C(5) -C(6) -C(7) -C(8) plane, phenyl ring are 31. 42 and 43. 78, respectively. The mor-pholine ring adopts chair conformation.展开更多
The title compound 2-(4-fluorophenylamino)-2-thiomethyl acetophe-none (C15H14FNOS, M. = 275. 34 ) was synthesized by the reaction of 2-hydroxy-2-thiomethyl acetohenone (abenzoylhemithioacetal ) with 4-fluoroaniline. T...The title compound 2-(4-fluorophenylamino)-2-thiomethyl acetophe-none (C15H14FNOS, M. = 275. 34 ) was synthesized by the reaction of 2-hydroxy-2-thiomethyl acetohenone (abenzoylhemithioacetal ) with 4-fluoroaniline. The crystal ismonoclinic, space group P21/n. with unit cell constants a = 12. 434 (4 ), b = 6. 00l2(6), c=l8. 49l(2) A, β=100. 87(l)° Z = 4, V = 1355. O(5) A, D'= 1. 350g/cm3, μ(MoKa) = 2. 41 cm-l, F(000) = 576, R=0. 029, Rw.= 0. 041 for 14l2 ob-served reflections (I> 3σ(I) ). X-ray analysis reveals that the dihedral angle betweenplane l (C(l)~C(6), F, N ) and plane 2 (C(8)~C(14), O ) is 4. l8° and theC(7) -S bond is longer than normal single C-S bond.展开更多
基金Supported by the National Natural Science Foundation of China(Nos.20772088,21172163)the Project Funded by the Priority Academic Program Development of Jiangsu Higher Education Institutions,China(No.JSSYSXK2010007)
文摘Ga（ClO4）3-catalyzed reaction of 1,2-aryldiamines and α-bromoketones to afford 2-substituted quinoxalines in good yields is described.The reaction proceeded via grinding process with 10%（molar fraction） catalyst under solvent-free conditions at room temperature.For unsymmetrical o-phenylenediamines bearing electron-withdrawing groups,regio-selective quinoxalines were obtained.
基金Supported by the National Natural Science Foundation of China under Grant No.59832100.
文摘A novel technique to extend template application ofanodic porous alumina to Si has been reported.First,porous alumina template about 400 nm thick was prepared on silicon substrate by anodizing thin aluminum film with high purity of 99.99%in 15 wt.%sulfuric acid under a constant voltage of 20 V and at an electrolyte temperature of 5°C.Then,amorphous Si layer approximately 50nm in thickness was deposited onto the surface of template by using electron beam evaporation technique followed by an Xe ion beam bombardment,upon which as-coated Si layer at the pore mouth could be removed into pores smootlly.Three runs were performed by repeating above process of deposition and post bombardment.Finally,samples were annealed at 800°C for 30min in nitrogen.Transmission electron microscopy and x-ray diffraction analysis reveal Si nanocrystals with a size of 15-20nm being formed in the pores of template.
基金The project was supported by the Key Laboratory of Organic Synthesis of Jiangsu Province (JSK016)
文摘The title compound 1,5-diphenyl-3-phenacylthio-1H-1,2,4-triazole 2 （C22H17- N3OS, Mr = 371.45） was prepared by the reaction of 1-benzoyl-3-phenyl-aminothiourea 1 with 2-bromoacetophenone. The crystal is of triclinic, space group P^1-, a = 8.906（3）, b = 9.853（3）, c = 11.226（4）A, α= 100.562（5）, β= 101.285（5）, γ. = 105.096（6）^c, Z = 2, V = 903.7（5） ]A^3, Dc= 1.365 g/cm^3,μ（MoKa） = 0.196 mm^-1, F（000） = 388, the final R = 0.0506 and wR = 0.0985 for 2532 observed reflections （I〉 2σ（I））. Its formation mechanism was proposed.
文摘,3-Disubstituted quinoxalines were synthesized from α-acetylthioformanilide and ophenylenediamine. Further studies sliowed that there existed competitive re- actions. One was a condensation reaction which produced substituted quinoxaline and the other was a substitution reaction which produced substituted quinoxaline-2- thione.
文摘The title compound 2, 3-diethoxycarbonyl-4-phenyl-5-morpholinylthiophene (C20H23NO5S, Mr=389. 47) was obtained by the reaction of a-thiobenzoylth-ioformmorpholine with diethyl acetylene dicarboxylate - The crystal is prismatic, spacegroup P1 ( 2), with unit cell constants 2337 observed reflections . X-ray analysis reveals that interatomic dis-tances for C(1 ) -C(2) and C(3) -C (4) are 1. 393 (4), 1. 370 (4) , respectively,which show that they are C=C double bond. The atoms of C(1 ), C(2), C(3), C(4)and S form a thiophene ring. The dihedral ang1es between thiophene ring and C(5) -C(6) -C(7) -C(8) plane, phenyl ring are 31. 42 and 43. 78, respectively. The mor-pholine ring adopts chair conformation.
文摘The title compound 2-(4-fluorophenylamino)-2-thiomethyl acetophe-none (C15H14FNOS, M. = 275. 34 ) was synthesized by the reaction of 2-hydroxy-2-thiomethyl acetohenone (abenzoylhemithioacetal ) with 4-fluoroaniline. The crystal ismonoclinic, space group P21/n. with unit cell constants a = 12. 434 (4 ), b = 6. 00l2(6), c=l8. 49l(2) A, β=100. 87(l)° Z = 4, V = 1355. O(5) A, D'= 1. 350g/cm3, μ(MoKa) = 2. 41 cm-l, F(000) = 576, R=0. 029, Rw.= 0. 041 for 14l2 ob-served reflections (I> 3σ(I) ). X-ray analysis reveals that the dihedral angle betweenplane l (C(l)~C(6), F, N ) and plane 2 (C(8)~C(14), O ) is 4. l8° and theC(7) -S bond is longer than normal single C-S bond.
