A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ...A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ratio of cyanuric chloride to hexane-1,6-diamine was 2:1,using sodium hydroxide as base and the mixture of dichlormethane and water as solvent.On the basis of these results,a L9(33) orthogonal layout was designed to investigate the effects of the reaction time,the variety and dosage of base as well as the vomule ratio of dichlormethane and water on the yields of products.Three levels were selected for every factor.The result showed that when the molar ratio of sodium hydroxide to hexane-1,6-diamine was 2:1,the volume ratio of dichloromethane and water was 1:1 and the reaction was carried out at 0-5 ℃ for 6 h,the product yield could reach to 92.8%.The structure of the target product was characterized by elementary analysis,MS,1 H-NMR and FTIR.展开更多
The compound [H2（teta）]2+·2Cl-·3H2O （teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis and the structure was determined by sin...The compound [H2（teta）]2+·2Cl-·3H2O （teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis and the structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic,space group Pī with a=7.8364（16）,b=8.3607（13）,c=9.4762（15）?,α=61.900（12）,β=78.970（16）,γ=80.008（16）°,V=535.06（16）?3,Z=1,ρcalc=1.277g/cm3,F（000）=226.The macrocylic tetraamine cation contains two protonated secondary amine N atoms and two secondary amine N atoms.The water molecules are distinguished by their inequality in structure formation.They are involved in different types of intermolecular hydrogen bonding in the crystal lattice.展开更多
The manganese(Ⅲ) complex [Mn (acacen) {N (CN)2}]n [H2acacen =bis (acetylacetone)ethylenediimine] has been synthesized and the structure has been determined. The complex forms a one-dimensional chain structure via the...The manganese(Ⅲ) complex [Mn (acacen) {N (CN)2}]n [H2acacen =bis (acetylacetone)ethylenediimine] has been synthesized and the structure has been determined. The complex forms a one-dimensional chain structure via the bidentate bridge ligandμ1,5-[N(CN)2]- linking [Mn(acacen)] moiety. The magnetic property of the compound (75～300 K) shows the existence of an antiferromagnetic exchange interaction among paramagnetic centers along the chain. CCDC: 244940.展开更多
叙述了以(4R) 羟基 (S) 脯氨酸为原料进行的几种新型手性催化剂的简便合成方法. (4S) 苯氧基 (S) 脯氨酸 1a由N 乙氧羰基 (4R) 羟基 (S) 脯氨酸甲酯经Mitsunobu反应, C 4构型发生翻转, 水解后得到; (4R) 芳甲氧基 (S) 脯氨酸由N 叔丁...叙述了以(4R) 羟基 (S) 脯氨酸为原料进行的几种新型手性催化剂的简便合成方法. (4S) 苯氧基 (S) 脯氨酸 1a由N 乙氧羰基 (4R) 羟基 (S) 脯氨酸甲酯经Mitsunobu反应, C 4构型发生翻转, 水解后得到; (4R) 芳甲氧基 (S) 脯氨酸由N 叔丁氧羰基 (4R) 羟基 (S) 脯氨酸用ArCH2X醚化后脱去N 保护基得到, C 4构型不受影响.展开更多
The cadmium complex[Cd(PMBP)2(EtOH)2](HPMBP =1-phenyl-3-methyl-4-benzoyl-pyrazolone-5)wassynthesized and characterized by IR and thermogravimetric analysis.The structure was determined by single X-ray diffraction anal...The cadmium complex[Cd(PMBP)2(EtOH)2](HPMBP =1-phenyl-3-methyl-4-benzoyl-pyrazolone-5)wassynthesized and characterized by IR and thermogravimetric analysis.The structure was determined by single X-ray diffraction anal-ysis.The crystal belongs to triclinic system,space group P 1.The crystallographic data are:a =9.121(4),b =10.193(5),c =10.895(5),α=107.085(4),β=108.239(4),γ=104.028(2)°,V=855.0(6) 3,Z =1,F(000) =390,Mr =759.12,Dc=1.474 Mg/m3,μ=0.692 mm-1,R1=0.0312 and wR2=0.0836.In the crystal Cd(Ⅱ)ion is coordinated by four oxygen atomsfrom two PMBP ligands and two oxygen atoms from two solvent EtOHmolecules to form a distorted octahedron geometry.展开更多
文摘A 1,3,5-triazin derivative: N,N’-bis-(4,6-dichloro——triazin-2-yl)-hexane-1,6-diamine was prepared from cyanuric chloride and hexane-1,6-diamine by nucleophilic substitution reaction.By trying experiments,the molar ratio of cyanuric chloride to hexane-1,6-diamine was 2:1,using sodium hydroxide as base and the mixture of dichlormethane and water as solvent.On the basis of these results,a L9(33) orthogonal layout was designed to investigate the effects of the reaction time,the variety and dosage of base as well as the vomule ratio of dichlormethane and water on the yields of products.Three levels were selected for every factor.The result showed that when the molar ratio of sodium hydroxide to hexane-1,6-diamine was 2:1,the volume ratio of dichloromethane and water was 1:1 and the reaction was carried out at 0-5 ℃ for 6 h,the product yield could reach to 92.8%.The structure of the target product was characterized by elementary analysis,MS,1 H-NMR and FTIR.
文摘The compound [H2（teta）]2+·2Cl-·3H2O （teta=meso-5,7,7,12,14,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane）was synthesized and characterized by elementary analysis and the structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic,space group Pī with a=7.8364（16）,b=8.3607（13）,c=9.4762（15）?,α=61.900（12）,β=78.970（16）,γ=80.008（16）°,V=535.06（16）?3,Z=1,ρcalc=1.277g/cm3,F（000）=226.The macrocylic tetraamine cation contains two protonated secondary amine N atoms and two secondary amine N atoms.The water molecules are distinguished by their inequality in structure formation.They are involved in different types of intermolecular hydrogen bonding in the crystal lattice.
文摘The manganese(Ⅲ) complex [Mn (acacen) {N (CN)2}]n [H2acacen =bis (acetylacetone)ethylenediimine] has been synthesized and the structure has been determined. The complex forms a one-dimensional chain structure via the bidentate bridge ligandμ1,5-[N(CN)2]- linking [Mn(acacen)] moiety. The magnetic property of the compound (75～300 K) shows the existence of an antiferromagnetic exchange interaction among paramagnetic centers along the chain. CCDC: 244940.
文摘叙述了以(4R) 羟基 (S) 脯氨酸为原料进行的几种新型手性催化剂的简便合成方法. (4S) 苯氧基 (S) 脯氨酸 1a由N 乙氧羰基 (4R) 羟基 (S) 脯氨酸甲酯经Mitsunobu反应, C 4构型发生翻转, 水解后得到; (4R) 芳甲氧基 (S) 脯氨酸由N 叔丁氧羰基 (4R) 羟基 (S) 脯氨酸用ArCH2X醚化后脱去N 保护基得到, C 4构型不受影响.
文摘The cadmium complex[Cd(PMBP)2(EtOH)2](HPMBP =1-phenyl-3-methyl-4-benzoyl-pyrazolone-5)wassynthesized and characterized by IR and thermogravimetric analysis.The structure was determined by single X-ray diffraction anal-ysis.The crystal belongs to triclinic system,space group P 1.The crystallographic data are:a =9.121(4),b =10.193(5),c =10.895(5),α=107.085(4),β=108.239(4),γ=104.028(2)°,V=855.0(6) 3,Z =1,F(000) =390,Mr =759.12,Dc=1.474 Mg/m3,μ=0.692 mm-1,R1=0.0312 and wR2=0.0836.In the crystal Cd(Ⅱ)ion is coordinated by four oxygen atomsfrom two PMBP ligands and two oxygen atoms from two solvent EtOHmolecules to form a distorted octahedron geometry.
