Eight novel Schiff Bases, from 6,6′-diformyl-2,2′-bipyridyl (1a, 43%)with O, N, S and F containing amines: Thiosemicarbazide (2a, 70%), 4-Ethyl-3-thiosemicabazide (2b, 75%), 4,4-Dimethyl-3-thio-semicarbazide (2c, 75...Eight novel Schiff Bases, from 6,6′-diformyl-2,2′-bipyridyl (1a, 43%)with O, N, S and F containing amines: Thiosemicarbazide (2a, 70%), 4-Ethyl-3-thiosemicabazide (2b, 75%), 4,4-Dimethyl-3-thio-semicarbazide (2c, 75%), S-benzyldithiocarbazide, SBDTC (2d, 80%), (Trifluromethyl) phenylhy-drazine (2e, 80%), 4-Phenyl-3-thiosemcarbazide (2f, 80%), Thiocarbazide (2g, 70%), 2-Amino-thiophenol (2h, 65%), have been synthesized. The conventional method of synthesis of the Schiff bases involves refluxing the reaction mixture containing the diformyls and amines for 1 hour. The solid products that had formed were filtered off using suction filtration. In few reactions, 2 - 3 drops of conc. sulfuric acid were used to obtain high yield. The structures of all eight novel synthesized compounds have fully been characterized by spectroscopic (IR, NMR, MS) methods.展开更多
Lithium aluminium amide [LiAI（NHR）4] 5 obtained by treating the primary amine 4 with LiAlH4 could promote the ring opening of epoxide 2 and led to high regioselective product of racemic bis[2-（6-fluoro-2-chromanyl...Lithium aluminium amide [LiAI（NHR）4] 5 obtained by treating the primary amine 4 with LiAlH4 could promote the ring opening of epoxide 2 and led to high regioselective product of racemic bis[2-（6-fluoro-2-chromanyl）-2-hydroxyethyl]amine methanesulfonic acid salt 7.展开更多
The title compound N-（（6-chloropyridin-3-yl）methyl）-6-ethoxy-N-ethyl-3-nitropyri-din-2-amine（4） was synthesized by reacting the mixture of 6-chloro-2-ethoxy-3-nitropyridine（1） and 2-chloro-6-ethoxy-3-nitropyri...The title compound N-（（6-chloropyridin-3-yl）methyl）-6-ethoxy-N-ethyl-3-nitropyri-din-2-amine（4） was synthesized by reacting the mixture of 6-chloro-2-ethoxy-3-nitropyridine（1） and 2-chloro-6-ethoxy-3-nitropyridine（2） with 3,and its structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 7.3441（2）,b = 9.9041（3）,c = 11.7368（3） ,α = 101.410（2）,β = 102.1340（10）,γ = 99.594（2）o,μ = 0.260 mm^-1,Mr = 336.78,V = 798.58（4）（A°）^3,Z = 2,Dc = 1.401g/cm^3,F（000） = 352,T = 296（2） K,R = 0.0210 and wR = 0.1053.展开更多
The title complex has been synthesized and its crystal structure was determined by X-ray diffraction. Prisms of Cd (C_(21)H_(24)N_4)(NO_3)_2(1) crystallize in the triclinic space group P with cell dimensions a= 8.112(...The title complex has been synthesized and its crystal structure was determined by X-ray diffraction. Prisms of Cd (C_(21)H_(24)N_4)(NO_3)_2(1) crystallize in the triclinic space group P with cell dimensions a= 8.112(1),b=8. 837(2), c=17.236(4),α=78. 80(2),β=89. 99(2),γ=74. 35(2)°,V=1167.4(6),Mr=568. 86, Z=2, F(000)=576,μ= 9.78 cm-1 and Dc= 1. 618 g/cm￣3. 2756 unique reflections with I≥3σ(I) on refinement afforded values of R=0. 047 and R_w=0. 055.The Cd(Ⅱ) atom is surrounded by three oxygen atoms from two nitrate groups and three nitrogen atoms from TLA ligand in a distorted octahedron.展开更多
文摘Eight novel Schiff Bases, from 6,6′-diformyl-2,2′-bipyridyl (1a, 43%)with O, N, S and F containing amines: Thiosemicarbazide (2a, 70%), 4-Ethyl-3-thiosemicabazide (2b, 75%), 4,4-Dimethyl-3-thio-semicarbazide (2c, 75%), S-benzyldithiocarbazide, SBDTC (2d, 80%), (Trifluromethyl) phenylhy-drazine (2e, 80%), 4-Phenyl-3-thiosemcarbazide (2f, 80%), Thiocarbazide (2g, 70%), 2-Amino-thiophenol (2h, 65%), have been synthesized. The conventional method of synthesis of the Schiff bases involves refluxing the reaction mixture containing the diformyls and amines for 1 hour. The solid products that had formed were filtered off using suction filtration. In few reactions, 2 - 3 drops of conc. sulfuric acid were used to obtain high yield. The structures of all eight novel synthesized compounds have fully been characterized by spectroscopic (IR, NMR, MS) methods.
基金the National 863 Program(No.2003AA323030)the National Natural Science Foundation of China(No.50272069 and No.20472090)for financial support.
文摘Lithium aluminium amide [LiAI（NHR）4] 5 obtained by treating the primary amine 4 with LiAlH4 could promote the ring opening of epoxide 2 and led to high regioselective product of racemic bis[2-（6-fluoro-2-chromanyl）-2-hydroxyethyl]amine methanesulfonic acid salt 7.
基金Supported by the National Basic Research Program of China (973 Program,2010CB126104)the NNSFC (Nos. 20572019 and 20872033)+3 种基金National Twelfth-five Key Project of China (Nos. 2011BAE06B01 and 2011BAE06B02)the NSF of Hunan Province (11JJ2006, 11JJ3022 and 10JJ3053)Science Plan of Hunan Province (2010FJ2003)research condition innovation of Hunan Province (2010PT2058)
文摘The title compound N-（（6-chloropyridin-3-yl）methyl）-6-ethoxy-N-ethyl-3-nitropyri-din-2-amine（4） was synthesized by reacting the mixture of 6-chloro-2-ethoxy-3-nitropyridine（1） and 2-chloro-6-ethoxy-3-nitropyridine（2） with 3,and its structure was determined by X-ray single-crystal diffraction.The crystal belongs to the monoclinic system,space group P21/n with a = 7.3441（2）,b = 9.9041（3）,c = 11.7368（3） ,α = 101.410（2）,β = 102.1340（10）,γ = 99.594（2）o,μ = 0.260 mm^-1,Mr = 336.78,V = 798.58（4）（A°）^3,Z = 2,Dc = 1.401g/cm^3,F（000） = 352,T = 296（2） K,R = 0.0210 and wR = 0.1053.
文摘The title complex has been synthesized and its crystal structure was determined by X-ray diffraction. Prisms of Cd (C_(21)H_(24)N_4)(NO_3)_2(1) crystallize in the triclinic space group P with cell dimensions a= 8.112(1),b=8. 837(2), c=17.236(4),α=78. 80(2),β=89. 99(2),γ=74. 35(2)°,V=1167.4(6),Mr=568. 86, Z=2, F(000)=576,μ= 9.78 cm-1 and Dc= 1. 618 g/cm￣3. 2756 unique reflections with I≥3σ(I) on refinement afforded values of R=0. 047 and R_w=0. 055.The Cd(Ⅱ) atom is surrounded by three oxygen atoms from two nitrate groups and three nitrogen atoms from TLA ligand in a distorted octahedron.
