A novel technique combining photoelectronic microscopy and computer imaging tracing was used to investigate the synthesis of thioether(2-[3-methyl-4-(2,2,2-trifluoro-ethoxy)-pyridine-2-(methylsulfanyl)]-1H-benzoimidaz...A novel technique combining photoelectronic microscopy and computer imaging tracing was used to investigate the synthesis of thioether(2-[3-methyl-4-(2,2,2-trifluoro-ethoxy)-pyridine-2-(methylsulfanyl)]-1H-benzoimidazole),which is an intermediate for lansoprazole.Visualization in sub-microcosmic surroundings was realized to study interfacial phenomenon.The reaction kinetics study by a visualization technique was carried out in a mini-reactor,and the concentration-gray scale standard curves for thioether were obtained by analyzing the gray scales of digital images.Based on the concentration-gray scale standard curves,the reactant concentrations at different times were calculated,and the reaction kinetics curve and reaction rate equation were obtained.Also the total mass-transfer resistance from bulk phase to interface of sodium imidazole and bromopyridine was obtained.Liquid-liquid interface of synthesizing thioether was observed and its mass transfer mechanism was discussed.展开更多
In situ metal/ligand reactions have been investigated for decades and turn out to be efficient for discovery of new organic reactions and coordination compounds with novel topology and functionalities. 4-[(2-Pyridin-2...In situ metal/ligand reactions have been investigated for decades and turn out to be efficient for discovery of new organic reactions and coordination compounds with novel topology and functionalities. 4-[(2-Pyridin-2-yl)-1-(pyridin-2-yl)vinylthio]benzoic acid(L) was in situ generated in solvethermal condition with CuO and CuBr2. A copper coordination polymer[Cu2(L)Br2]n(1) was obtained synchronously and characterized by X-ray single crystal diffraction,elemental analysis and FTIR spectrum. The Cu+ ions were bridged into a tetranuclear cluster by μ3-Br and μ2-Br ions,and the clusters were further linked into 1D ribbon-like chain. The intermolecular in situ elimination is rare but meaningful in the synthesis of organic compounds.展开更多
An efficient and environmental-friendly one-pot procedure has been developed for the synthesis of 1,3,4-oxadiazole-5- thioethers by the reaction of acylhydrazine with carbon disulfide and organic halides or α, β-uns...An efficient and environmental-friendly one-pot procedure has been developed for the synthesis of 1,3,4-oxadiazole-5- thioethers by the reaction of acylhydrazine with carbon disulfide and organic halides or α, β-unsaturated carbonyl compounds. The reactions were carried out in water in the presence of potassium phosphate within 2-4 h to afford the expected products in excellent yields.展开更多
A five-membered phosphoroheterocycle, 5, 5-dimethyl-2-(4 -methoxy)phenyl-1, 3, 2-thiazaphospholidine-4-thione 2-sulfide, has been prepared by the reaction of Lawessons reagent (LR) with -hydroxyl isobutyronitrile, and...A five-membered phosphoroheterocycle, 5, 5-dimethyl-2-(4 -methoxy)phenyl-1, 3, 2-thiazaphospholidine-4-thione 2-sulfide, has been prepared by the reaction of Lawessons reagent (LR) with -hydroxyl isobutyronitrile, and its crystal structure was determined by X-ray diffraction method. The title compound (C11H14NOPS3) is triclinic with space group P , a= 6.8418 (9), b= 10.5467 (1), c= 11.5670 (2)? = 114.851 (2),β= 100.291 (2),γ= 91.390 (3)? V= 740.7 (2) 3, Z= 2, Dc= 1.360 g/cm3, λ= 0.71073 ? μ(MoK?= 0.59 mm-1, F(000)= 316. The Structure was refined to R= 0.0476, wR= 0.1272 for 2549 unique reflections with I >2σ(I). It contains a phenyl ring and a 5-membered phosphoroheterocycle with the dihedral angle of 87.06 (9)? The five atoms (P (1), N (1), C (1), C (2) and S (2)) of the heterocycle are nearly coplanar. In view of the unit cell it can be concluded that there exists an intermolecular hydrogen bond in the form of Sa┈HN (a: X, Y+1,Z+1). The existence of dpлbond between P (1) and N (1) was found as well as unsaturated property of N (1)C (1) moiety.展开更多
Network crewn ether polymer with pendant sulfide side ohain in the networkstructure units has been synthesized via ring- opening copolymerization of β-ethylthioethyl glycidyl ether and diethylene glycol bisglycidyl e...Network crewn ether polymer with pendant sulfide side ohain in the networkstructure units has been synthesized via ring- opening copolymerization of β-ethylthioethyl glycidyl ether and diethylene glycol bisglycidyl ether. A kind of active catalyst suitable for this reaction was suggested. The title polymer was found tobe a good ligand for platinous chloride, and the platinous complex could catalyze thehydrosilylation of olefins with triethoxysilane efficiently.展开更多
C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051...C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051(0.057) for 1446 observed reflections with I≥3σ(Ⅰ).The sulfur-sulfur bond length is found to be 2. 019(2) A with a dihedral angle CSSC of 93.29°.展开更多
文摘A novel technique combining photoelectronic microscopy and computer imaging tracing was used to investigate the synthesis of thioether(2-[3-methyl-4-(2,2,2-trifluoro-ethoxy)-pyridine-2-(methylsulfanyl)]-1H-benzoimidazole),which is an intermediate for lansoprazole.Visualization in sub-microcosmic surroundings was realized to study interfacial phenomenon.The reaction kinetics study by a visualization technique was carried out in a mini-reactor,and the concentration-gray scale standard curves for thioether were obtained by analyzing the gray scales of digital images.Based on the concentration-gray scale standard curves,the reactant concentrations at different times were calculated,and the reaction kinetics curve and reaction rate equation were obtained.Also the total mass-transfer resistance from bulk phase to interface of sodium imidazole and bromopyridine was obtained.Liquid-liquid interface of synthesizing thioether was observed and its mass transfer mechanism was discussed.
文摘In situ metal/ligand reactions have been investigated for decades and turn out to be efficient for discovery of new organic reactions and coordination compounds with novel topology and functionalities. 4-[(2-Pyridin-2-yl)-1-(pyridin-2-yl)vinylthio]benzoic acid(L) was in situ generated in solvethermal condition with CuO and CuBr2. A copper coordination polymer[Cu2(L)Br2]n(1) was obtained synchronously and characterized by X-ray single crystal diffraction,elemental analysis and FTIR spectrum. The Cu+ ions were bridged into a tetranuclear cluster by μ3-Br and μ2-Br ions,and the clusters were further linked into 1D ribbon-like chain. The intermolecular in situ elimination is rare but meaningful in the synthesis of organic compounds.
基金Natural Science Foundation of China (Grant No.20672009)the Major State Basic Research Development Program(Grant No.2004CB719900).
文摘An efficient and environmental-friendly one-pot procedure has been developed for the synthesis of 1,3,4-oxadiazole-5- thioethers by the reaction of acylhydrazine with carbon disulfide and organic halides or α, β-unsaturated carbonyl compounds. The reactions were carried out in water in the presence of potassium phosphate within 2-4 h to afford the expected products in excellent yields.
文摘A five-membered phosphoroheterocycle, 5, 5-dimethyl-2-(4 -methoxy)phenyl-1, 3, 2-thiazaphospholidine-4-thione 2-sulfide, has been prepared by the reaction of Lawessons reagent (LR) with -hydroxyl isobutyronitrile, and its crystal structure was determined by X-ray diffraction method. The title compound (C11H14NOPS3) is triclinic with space group P , a= 6.8418 (9), b= 10.5467 (1), c= 11.5670 (2)? = 114.851 (2),β= 100.291 (2),γ= 91.390 (3)? V= 740.7 (2) 3, Z= 2, Dc= 1.360 g/cm3, λ= 0.71073 ? μ(MoK?= 0.59 mm-1, F(000)= 316. The Structure was refined to R= 0.0476, wR= 0.1272 for 2549 unique reflections with I >2σ(I). It contains a phenyl ring and a 5-membered phosphoroheterocycle with the dihedral angle of 87.06 (9)? The five atoms (P (1), N (1), C (1), C (2) and S (2)) of the heterocycle are nearly coplanar. In view of the unit cell it can be concluded that there exists an intermolecular hydrogen bond in the form of Sa┈HN (a: X, Y+1,Z+1). The existence of dpлbond between P (1) and N (1) was found as well as unsaturated property of N (1)C (1) moiety.
文摘Network crewn ether polymer with pendant sulfide side ohain in the networkstructure units has been synthesized via ring- opening copolymerization of β-ethylthioethyl glycidyl ether and diethylene glycol bisglycidyl ether. A kind of active catalyst suitable for this reaction was suggested. The title polymer was found tobe a good ligand for platinous chloride, and the platinous complex could catalyze thehydrosilylation of olefins with triethoxysilane efficiently.
文摘C_(10)H_8N_2O_2S_2, Mr=252. 32,monoclinic,P2_(1/c),a=7.165(5).b=7.659(3),c=19.543(8)A,β=96. 76(5)°,V=1065.0(9) A,Z=4,D_c=1. 57 g/cm￣3.The structure was solved by direct methods and refined to final R(R_w)=0.051(0.057) for 1446 observed reflections with I≥3σ(Ⅰ).The sulfur-sulfur bond length is found to be 2. 019(2) A with a dihedral angle CSSC of 93.29°.
