含吡唑环的双杂环化合物的合成及其生物活性

以4-硝基-5-吡唑甲酰肼为起始物,合成了一系列含硝基的5-吡唑基-1,3,4-噁二唑类、5-吡唑基-1,3,4-噻二唑类和5-吡唑基-1,3,4-三唑类的化合物.初步生测结果表明:部分化合物有较好的杀菌和内吸活性.     

2-取代-5-吡唑基-1，3，4-恶二唑类化合物的合成及生物活性

以5-吡唑甲酰肼和取代羧酸为起始物,运用"一锅煮"法合成了一系列2-取代-5-吡唑基-1,3,4-二唑.此外,还合成了1-苯酰基-2-吡唑酰基肼.初步生物活性测定结果表明,部分化合物有较好的杀菌和除草活性.     

2-(1-苯基-3-芳基吡唑-4-基)-3-芳酰氨基-4-噻唑啉酮的合成

1-苯基-3-芳基-4-甲酰基吡唑与芳酰肼在乙醇中回流,缩合所得的腙在巯基乙酸作用下,合环得到2-(1-苯基-3-芳基吡唑-4-基)-3-芳酰氨基-4-噻唑啉酮类化合物,其结构经IR,MS,1HNMR谱和元素分析确证。     

新型5-芳甲酰胺基-6-芳胺基-吡唑并[3,4-d] 嘧啶-4-酮衍生物的合成及其除草活性

以吡唑膦亚胺、芳基异氰酸酯和芳基甲酰肼为原料，通过串联氮杂Wittig反应关环合成了12种新型的5-芳甲酰胺基-6-芳胺基-吡唑并[3,4-d]嘧啶-4-酮衍生物(3a~3l)，其结构经¹H NMR, ¹³C NMR， IR和HR-MS(ESI)表征。对单双子叶除草活性的初步测试结果发现：部分化合物具有优异的除草活性，特别是浓度为100 mg·L^-1时，5-(4-氟苯甲酰胺基)-6-(4-氯苯胺基)-3-甲硫基-1-苯基-1H-吡唑[3,4-d]-嘧啶-4(5H)-酮3i和5-(4-吡啶苯甲酰胺基)-6-(4-氯苯胺基)-3-甲硫基-1-苯基-1H-吡唑[3,4-d]-嘧啶-4 (5H)-酮3k对油菜和稗草的茎和根的抑制率高达100%。     

2,5-二取代基-1,3,4-噁二唑及噁二唑啉类化合物的合成

2-苯基-1,2,3-连三唑-4-甲酰肼(1)与芳酸在POCl_3催化下得到6种新的2-芳基-5-(2’-苯基-1’,2’,3’-连三唑-4’-基)-1,3,4-噁二唑(2)。1与羰基化合物缩合得到相应的酰腙(3),在Ac_2O作用下环化成2-取代基-3-乙酰基-5-(2’-苯基-1’,2’,3’-连三唑-4’-基)-1,3,4-噁二唑啉(4)。化合物的结构经元素分析,IR,~1H NMR和MS确证。     

1-芳酰基-4-(5-芳基-2-呋喃甲酰基)氨基硫脲衍生物的合成及其生物活性

酰胺基硫脲;芳基酰肼;1-芳酰基-4-(5-芳基-2-呋喃甲酰基)氨基硫脲衍生物的合成及其生物活性     

In(Ⅲ)-1-苯基-3-甲基-4-噻吩甲酰基-吡唑啉酮-5配合物吸附波的研究

在pH3.0的HCl-NaAc介质中,In(Ⅲ)与1_苯基_3_甲基_4_噻吩甲酰基_吡唑啉酮_5(HPMTHP)生成配合物,于-0.63V(vs.SCE)处出现一尖锐、灵敏的极谱峰,In含量在0.002～1μg/mL范围内与峰高呈线性关系。用多种电化学方法研究了极谱波的性质及反应机理,证明-0.63V处的极谱波为配合物吸附波,峰电流由中心离子In(Ⅲ)还原产生。用直线法测得配合物组成为n[In(Ⅲ)]∶n(HPMTHP)=1∶1,表观稳定常数为2.96×103。     

铽(Ⅲ)-1,4-双(1′-苯基-3′-甲基-5′-氧代吡唑-4′-基)丁二酮-[1,4]体系荧光性质的研究及应用

本文研究了Tb(Ⅲ)-1,4-双(′-苯基-3′-甲基-5′-氧代吡唑-4′-基)丁二酮-[1,4](BPMPBD)-溴化十六烷基三甲胺(CTMAB)体系的荧光性质,探讨了响影体系荧光性质的诸因素,确定了最佳实验条件。该体系中Tb(Ⅲ)浓度以2.0×10~(-5)～1.0×10~(-10)mol/L范围内与其荧光强度呈线性关系,检测限可达到5.0×10~(-11)mol/L。应用于合成样品中微量Tb(Ⅲ)的分析,结果令人满意。     

1-[6-(3,5-二甲基-1H-吡唑-1-基)-1,2,4,5-四嗪-3-基]酰肼及其衍生物的合成与表征

以水合肼和硝酸胍为原料,经肼化、环化、氧化和肼化四步反应合成了1-[6-(3,5-二甲基-1H吡唑-1-基)-1,2,4,5-四嗪-3-基]酰肼(4);4与酰氯或磺酰氯反应合成了一系列新型的1-[6-(3,5-二甲基-1H-吡唑-1-基)-1,2,4,5-四嗪-3基]酰肼衍生物(6a～6j),其结构经1H NMR,IR...     

微波促进下1-芳甲酰基-4-(2′-苯并呋喃甲酰基)氨基硫脲及其衍生物的合成

微波辐射条件下 ,首先由 2 苯并呋喃甲酰氯在相转移条件下依次与硫氰酸铵和芳甲酰肼反应合成了一系列 1 芳甲酰基 4 ( 2′ 苯并呋喃甲酰基 )氨基硫脲 .进一步在微波辐射的条件下由这些氨基硫脲分别与碘酸钾、醋酸或醋酸汞等试剂作用高产率地制得了 1 芳甲酰基 4 ( 2′ 苯并呋喃甲酰基 )氨基脲、2 芳基 5 ( 2′ 苯并呋喃甲酰胺基 ) 1,3 ,4 噻二唑和 2 芳基 5 ( 2′ 苯并呋喃甲酰胺基 ) 1,3 ,4 二唑 .     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]lisoindol-2(1H)-yl]-3-(trifluoromethyl)phenylmethanimine

The crystal structure of the title compound (C19H15F3N2O2, Mr= 360.33) was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P(1), with a = 6.5604(7), b = 13.9614(16), c = 18.1790(18) (A), α = 102.749(7),β = 97.542(6), γ = 94.355(4)°, V= 1600.5(3) (A)3, Z = 4, Dc = 1.495 g/cm3, λ(MoKα) = 0.71070, F(000) = 744, μ(MoKα) = 0.122mm-1, R = 0.0434 and wR = 0.1051. A total of 7590 unique reflections were collected, of which 5429 with |F|2 ≥ 2σ|F|2 were observed. The two cyclohexene rings in the molecule adopt boat-boat conformations with the deviations of ring atoms C(9) and C10 from the C(5)/C(6)/C(7)/C(8) plane (Ⅰ) by 1.1204 (0.0023) and 1.1132 (0.0023) (A), respectively, whereas from the C(2)/C(3)/C(5)/C(8)plane (Ⅱ) by 1.1627 (0.0022) and 1.1818 (0.0021) (A), respectively. In the cyclopropane and lactam rings, atoms C(11) and N(1) point towards the double bond of C(9)-C(10) and the dihedral angle between the ring plane (Ⅲ) containing C(1), C(2), C(3) and C(4) and plane (Ⅳ) consisting of C(6),C(7) and C(11) is 55.76 (0.07)°. The dihedral angles between planes Ⅳ and Ⅰ and Ⅱ and Ⅲ are 63.58 (0.07)° and 58.10 (0.06)°, respectively. The dihedral angle between the benzene ring C(13)～C(18) and plane Ⅳ is 42.41 (0.06)°.     

Synthesis and Crystal Structure of N-[（3aR,4R,4aR,5aS,6S,6aS）-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]isoindol-2（1H）-yl]-3-（trifluoromethyl）phenylmethanimine

The crystal structure of the title compound(C19H15F3N2O2,Mr = 360.33) was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic,space group P1,with a = 6.5604(7),b = 13.9614(16),c = 18.1790(18) ,α = 102.749(7),β = 97.542(6),γ = 94.355(4)°,V = 1600.5(3) 3,Z = 4,Dc = 1.495 g/cm3,λ(MoKα) = 0.71070,F(000) = 744,μ(MoKα) = 0.122 mm-1,R = 0.0434 and wR = 0.1051.A total of 7590 unique reflections were collected,of which 5429 with |F|2 ≥ 2σ|F|2 were observed.The two cyclohexene rings in the molecule adopt boat-boat conformations with the deviations of ring atoms C(9) and C10 from the C(5)/C(6)/C(7)/C(8) plane(Ⅰ) by 1.1204(0.0023) and 1.1132(0.0023) ,respectively,whereas from the C(2)/C(3)/C(5)/C(8) plane(Ⅱ) by 1.1627(0.0022) and 1.1818(0.0021) ,respectively.In the cyclopropane and lactam rings,atoms C(11) and N(1) point towards the double bond of C(9)-C(10) and the dihedral angle between the ring plane(Ⅲ) containing C(1),C(2),C(3) and C(4) and plane(IV) consisting of C(6),C(7) and C(11) is 55.76(0.07)°.The dihedral angles between planes Ⅳ and Ⅰ and Ⅱ and Ⅲare 63.58(0.07)° and 58.10(0.06)°,respectively.The dihedral angle between the benzene ring C(13)～ C(18) and plane Ⅳ is 42.41(0.06)°.     

Syn thesis,Characterization of 1,3-Diisopropoxyaloxanes,Their Modification on Calcium Carbonate Filler

Five 1,3-diisopropoxyaloxanes, i. e., (PrⁱO)RO₂AlOAlO₂R(OPrⁱ) [where R=C₁₆H₃₁(Ⅰ)_C₁₈H₃₅(Ⅱ), _C₉H₁₆CH=CHC₇H₁₅(Ⅲ), _P(OCH₂(C₂H₅)CHC₄H₉)₂(Ⅳ), and _C₁₂H₂₃(Ⅴ), respectively] were syn thesized by the hydrolysiscondensation of aluminium isopropoxide with water, exchange reaction with relevant acids. They were characterized by elemental analysis, determination of molecular weight, IR,, ²⁷Al NMR. The results show that the coordination number of Al atom in the compounds is 5, they exist in monomers in benzene. The analyses of TG/DTG, DTA indicated that both the thermal hydrolysis stability, thermal stability of these compounds are in the following order:Ⅰ<Ⅱ<Ⅲ<Ⅳ. The viscosity determinations of light calcium carbonate(L-CaCO₃)/liquid paraffin suspension systems demonstrated that they had an excellent modification effect on the surface of LCaCO₃ filler, the amount needed to form a monomolecular film on the surface of LCaCO₃ particles is in the order:Ⅰ<Ⅱ<Ⅲ<Ⅳ.     

3-甲基-5-氰基-6-氨基-1-苯基-4-(3,4-二甲氧基苯基)-1,4-二氢吡喃[2,3-c]吡唑的合成和晶体结构

标题化合物C22H20N4O3 3是由2-氰基-3-(3,4-二甲氧基苯基)丙烯腈1和3-甲基-1-苯基-2-吡唑-5-酮2在KF-Al2O3催化下在N,N-二甲基甲酰胺(DMF)溶剂中反应而得。结构通过单晶X-射线衍射分析确定,其晶体属于三斜晶系,空间群Pī,a = 9.450(3),b = 10.876(2), c = 11.435(2) ,a = 115.51(1), b = 102.82(1),g = 98.47(2), Mr = 388.42, V = 994.1(3) 3,Dc = 1.298 g/cm3, Z = 2, m (MoKa) = 0.089 mm-1, F(000) = 408。晶体结构用直接法解出,使用全矩阵最小二乘法对原子参数进行修正,最后的偏离因子R = 0.0420,wR = 0.1070。单晶X-射线衍射分析表明平面Ⅰ与平面Ⅱ、平面Ⅲ、平面Ⅳ的夹角分别为102.31、29.24和1.43。平面Ⅱ与平面Ⅲ和平面Ⅳ的夹角分别为73.50和100.91,平面Ⅲ和平面Ⅳ的夹角为27.81, 另外晶体中还存在分子间氢键。     

Synthesis and Structure of 6-(4-Fluorobenzylamino)-3-methylthio-1,5-diphenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one

1 INTRODUCTION It was reported that the pyrazolopyrimidinone derivatives play a very important role in the bio- chemistry of living cell. Many potential drugs[1～3] and agrochemicals[4, 5] have been modeled on the compound, and the study on derivatives …     

硫氰化铵-溴化十六烷基吡啶体系浮选分离和富集锗

研究了硫氰化铵-溴化十六烷基吡啶(CPB)体系浮选分离锗的行为及与一些金属离子分离的条件。结果表明,在水溶液中,Ge(Ⅳ)与硫氰化铵和溴化十六烷基吡啶形成不溶于水的三元缔合物[Ge(SCN)62-][CPB+]2,此三元缔合物沉淀浮于水相上层形成界面清晰的液-固两相。当溶液中溴化十六烷基吡啶和硫氰化铵的浓度分别为3.0×10-3mol/L和1.5×10-2mol/L时,Ge(Ⅳ)可与Ga(Ⅲ)、Ni(Ⅱ)、Cd(Ⅱ)、Mg(Ⅱ)、Mn(Ⅱ)、Fe(Ⅱ)、Al(Ⅲ)、Cr(Ⅲ)和V(Ⅴ)离子定量分离,Ge(Ⅳ)的浮选率达到98.3%以上。对合成水样中Ge(Ⅳ)的分离和测定,结果满意。该方法在微量锗的分离和富集分析中有一定的实用价值。     

4-氟-1,2-二氢-3,6-哒嗪二酮及其衍生物的合成

本文报导了4-氟-1,2-二氢-3,6-哒嗪二酮(Ⅱ)及其衍生物3,6-二氯-4-氟哒嗪(Ⅲ)、3-甲氧基-4-氟-6-氯哒嗪(Ⅳ)、3-邻甲苯氧基-4-氟-6-氯哒嗪(Ⅵ)、1-苯基-3-羟基-4-氟-6-哒嗪酮(Ⅶ)等五种新化合物的合成,探讨了(Ⅲ)同亲核试剂的反应性能和部分化合物的药理实验结果.     

KBr-乙醇-(NH_4)_2SO_4体系析相萃取分离和富集铱的研究

研究了KBr-乙醇-(NH_4)_2SO_4水体系析相萃取分离和富集铱的行为及与一些金属离子分离的条件.结果表明,(NH_4)_2SO_4能使乙醇的水溶液分成两相,在分相过程中,Ir(Ⅳ)与KBr生成的IrBr_6~(2-)与质子化乙醇(C_2H_5OH~(2+))形成的缔合物[IrBr_6~(2-)][C_2H_5OH~(2+)]_2能被乙醇相完全萃取.当乙醇、KBr和(NH_4)_2SO_4分别为体积分数30%、4.0×10~(-3)mol/J L、0.3 g,mL.pH 3时,Ir(Ⅳ)的萃取率达到99.5%以上,Ga(Ⅲ),Al(Ⅲ),Cr(Ⅲ),Mo(Ⅵ),Fe(Ⅲ),Ni(Ⅱ),Zn(Ⅱ),Co(Ⅱ),Mn(Ⅱ),V(Ⅴ),Ag(Ⅰ),Ru(Ⅲ)和Rh(Ⅲ)基本不被萃取,实现了Ir(Ⅳ)与上述金属离子的分离.     

稀土冠醚络合物的研究(Ⅲ)——轻稀土及钇的硝酸盐与2,3,11,12-四苯基-1,4,7,10,13,16-六氧-2,11-十八环二烯的络合物的合成及性质的研究

由三价轻稀土、钇(Ⅲ)和铈(Ⅳ)的硝酸盐分别与2,3,11,12-四苯基-1,4,7,10,13,16-六氧-2,11-十八环二烯反应,合成了相应的六种固体络合物,並进行了元素分析,IR、NMR、TG、DTA、电导及溶解度等性质的研究。     

4-氟-3-羟基-1-取代苯基-6-哒嗪酮及其衍生物的合成

报导4-氟-3-羟基-1-取代苯基-6-哒嗪酮及其衍生物的合成,氟代顺丁烯二酸酐和取代苯肼类反应的研究结果及部分化合物的药理实验结果。