N-[(吡啶-3-基)亚甲基]-4-氨基苯甲酰胺的合成及晶体结构

以对硝基苯甲酸为起始原料,经氯代、氨解、还原合成了N-[(吡啶-3-基)亚甲基]-4-氨基苯甲酰胺。通过熔点、元素分析、IR、1H NMR对其进行表征。利用Fe粉/醋酸和铁(Ⅱ)酞菁/NaBH4两种还原法,将中间产物分子中的硝基选择性还原为氨基,同时分子内的酰胺键不受影响,并获到了较高的收率。X-射线单晶衍射测定了其晶体结构,结果表明它属于单斜晶系,P21空间群,晶胞参数为:a=0.6324(8)nm,b=0.8739(11)nm,c=1.0281(12)nm,β=91.79(2)°,Z=2,V=0.5679(12)nm3,Dc=1.329g.cm-3,F(000)=240,μ=0.088mm-1,R1=0.0761,WR2=0.2120,S=1.044。     

1-[(乙氧基)甲基]-6-(1-萘甲基)胸腺嘧啶的合成

HEPT是抑制HIV-1逆转录酶的潜在活性化合物。1-[(乙氧基)甲基]-6-(1-萘甲基)胸腺嘧啶是HEPT的类似物,通过增加6位取代基的位阻可提高药效。文献设计并合成了该化合物,并对关键中间体(d)的合成及脱羟基反应作了初步讨论。     

2-[(4-羟基苯基)砜基]苯酚的合成及其精制新工艺

2-[(4-羟基苯基)砜基]苯酚的合成及其精制新工艺; [(羟基苯基)砜基]苯酚;苯酚;亚磷酸;偏三甲苯     

4-(6-甲氧基-2-萘基)-2-(2-羟苄亚氨基)噻唑合成与表征

6-甲氧基-2-(2-溴酰基)萘与硫脲反应环合得4-(6-甲氧基-2-萘基)-2-氨基噻唑;后者与水杨醛反应制备了新化合物4-(6-甲氧基-2-萘基)-2-(2-羟苄亚氨基)噻唑,收率为72.1%～94.8%.目标物采用核磁共振、红外光谱和元素分析测试技术进行了表征;分析目标物和中间体中萘环质子偶合分裂情况.并且确定了萘环上各质子的归属.     

多亚甲基桥连双(2-氨基-5-甲基-1,3,4-噻二唑)化合物的合成与表征

通过２－氨基－５－甲基－１,３,４－噻二唑与对甲基苯磺酰氯反应后再与多亚甲基双澳反应得到新化合物（１ａ～１ｅ）,１ａ～１ｅ醇解得５个新标题化合物。并由元素分析、ＩＲ和１ＨＮＭＲ确定了所有新化合物的结构。     

3,4-二甲氧基-6-氨基苯甲醛的合成

以藜芦醛为原料合成4,5-二甲氧基-2-硝基苯甲醛,经铁粉还原后高产率地得到了3,4-二甲氧基-6-氨基苯甲醛。     

Schiff碱N-(4-羟基苯基亚甲基)-对甲氧基苯胺的室温固相合成及表征

对甲氧基苯胺与对羟基苯甲醛通过室温固相反应一步合成N-(4-羟基苯基亚甲基)-对甲氧基苯胺(C14H13NO2),反应在15 min内完成,产率93%,分别用元素分析、红外光谱、X射线粉末衍射谱和核磁共振氢谱对产物进行了表征.     

2-[(4-氯苯基亚氨基)甲基]-8-羟基喹啉质子转移的理论研究

研究了2-[(4-氯苯基亚氨基)甲基]-8-羟基喹啉的三种质子转移途径: 分子内质子转移、水分子辅助质子转移和甲醇分子辅助质子转移. 以该席夫碱化合物的晶体结构作为模型, 在B3LYP/6-31＋G(d)水平上, 优化得到稳定态和过渡态的几何构型. 对三类质子转移前后的结构、能量、红外光谱、化学位移进行研究, 结果表明水分子辅助质子转移和甲醇分子辅助质子转移中, 水和甲醇分子利用氢键作用参与质子转移过程, 形成七元环状过渡态, 大大降低了反应的能垒, 有利于质子的转移, 氢键在降低活化能方面起着重要作用.     

8-溴-6-甲基-2-(1-吡咯烷基羰基)咪唑并[1,2-a]吡啶的合成及晶体结构

以2-氨基-5-甲基吡啶为原料,经溴代、环合、水解及酰胺化反应合成了8-溴-6-甲基-2-(1-吡咯烷基羰基)咪唑并[1,2-a]吡啶,总收率32.82％,其结构经1H-NMR和MS确证,并用X-单晶衍射法测定了其晶体结构.结果表明:待测物块状晶体a(CCDC:2039002)属三斜晶系,空间群P-1,晶胞参数a=6....     

2-[2'-(6'-甲氧基-苯并噻唑)偶氮]-5-二甲氨基苯甲酸的合成及其与Cu(Ⅱ)显色反应研究

报道了新试剂2-[2’-(6’-甲氧基-苯并噻唑)偶氮]-5-二甲氨基苯甲酸(简称MOBTAB)并研究了其在乙醇介质中与Cu(Ⅱ)的显色反应,试验表明,在pH2.0～4.5时,Cu(Ⅱ)与MOBTAB形成1:1的蓝色络合物.其最大吸收波长为670nm,表观摩尔吸光系数为6.55×10~4,Cu(Ⅱ)浓度在0～0.76μg·ml~(-1)范围内符合比耳定律.本法操作简便,可直接测定铸铝及纯铝中微量铜,结果满意.     

Synthesis, Crystal Structure and Fungicidal Activity of (E)-2-[(4-tert-Butyl-5- (4-methoxybenzyl)thiazol-2-ylimino)methyl]phenol

The title compound(E)-2-(4-tert-butyl-5-(4-methoxybenzyl)thiazol-2-ylimino)me-thylphenol was synthesized by the reaction of 5-(4-methoxybenzyl)-4-tert-butylthiazol-2-amine with salicylaldehyde=and its crystal structure was determined by single-crystal X-ray diffraction.The crystal belongs to the monoclinic system=space group P21/c with a=5.9362(8)=b=11.5070(15)=c=29.460(4)=β=97.326(3)°=V=1995.9(5)3=Z=4=F(000)=808=C22H24N2O2S=Mr=380.49=Dc=1.266 g/cm3=S=1.031=μ=0.181 mm--1=the final R=0.0474 and wR=0.1441 for 4327 observed reflections(I > 2σ(I)).Intramolecular O-H…N hydrogen bond is observed in the crystal.The preliminary bioassay showed that the title compound exhibits 95% inhibition rate against Rhizoctonia solani at the test concentration of 500 mg/L.     

Synthesis and characterization of oligo-4-[(pyridin-3-ylimino)methyl]phenol

The oxidative polycondensation of 4-[(pyridin-3-ylimino)methyl]phenol (4-PIMP) with O₂, H₂O₂, and NaOCl was studied in an aqueous alkaline medium between 50°C and 90°C. Oligo-4-[(pyridin-3-ylimino)methyl]phenol (O-4-PIMP) prepared was characterized by ¹H-NMR, ¹³C-NMR, FT-IR, UV-VIS, size-exclusion chromatography, and elemental and thermal analyses techniques. At the optimum reaction conditions, the yield of O-4-PIMP was 18.9%, 39.4%, and 46.8% using H₂O₂, O₂, and NaOCl oxidant, respectively. According to the TG analysis, the initial degradation temperature of O-4-PIMP was 218°C, which was by 50°C higher than that of 4-PIMP. Thermal analyses of 4-PIMP and O-4-PIMP were carried out in N₂ atmosphere at 15–1000°C. The highest occupied molecular orbital, the lowest unoccupied molecular orbital, and electrochemical energy gaps of 4-PIMP and O-4-PIMP were determined from the onset potentials for n-doping and p-doping, respectively. Also, optical band gaps of 4-PIMP and O-4-PIMP were determined according to UV-VIS measurements.     

Synthesis and Crystal Structure of （Z）-Methyl-3-methoxy-2-{2-[（4-（E-3-p-tolylacryloyl）phenoxy）methyl]phenyl}acrylate

The title compound,(Z)-methyl-3-methoxy-2-{2-[(4-(E-3-p-tolylacryloyl)phenoxy)-methyl]phenyl}acrylate,was synthesized and determined by X-ray single-crystal diffraction. The crystal belongs to the triclinic system,space group P1 with a = 8.0157(8),b = 12.5748(13),c = 13.3768(14) ,α = 64.770(2),β = 75.720 (2),γ = 89.784(2)°,μ = 0.085 mm-1,Mr = 442.49,V = 1174.1(2) 3,Z = 2,Dc = 1.252 g/cm3,F(000) = 468,T = 294(2) K,R = 0.0603 and wR = 0.1498 for 2644 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the single crystal contains strong non-classical hydrogen bonds. The preliminary bioassay showed that the title compound exhibits inhibitory activity against the Pseudoperoniospora cubensis and Rhizoctonia solani at the test concentration of 200 mg/L.     

Synthesis and Crystal Structure of 2-[（4-Methoxy- 6-methylthio-2-pyrimidinyl）aminocarbonyl- aminosulfonyl] Benzoic Acid Methyl Ester

1 INTRODUCTION The sulfonylurea herbicides are characterized by broad-spectrum weed control at very low use rates (c.2~75g ai ha-1), good crop selectivity and very low acute and chronic animal toxicity (acute oral LD50 to rat >4000 mg/kg)[1]. They are e…     

2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-5-(取代苯基亚甲基)-4- 噻唑啉酮的合成

以2-氨基-5-取代苯氧甲基-1,3,4-噻二唑(1)为起始原料, 合成了中间体2-氯乙酰氨基-5-取代苯氧甲基-1,3,4-噻二唑)-2-乙酰亚胺(2)和2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-4-噻唑啉酮(3), 化合物3进一步与取代苯甲醛发生类Knoevenagle缩合反应, 得到了一系列2-(5-取代苯氧甲基-1,3,4-噻二唑-2-亚胺基)-5-(取代苯基亚甲基)-4-噻唑啉酮类化合物4a～4p. 目标化合物4a～4p的结构经IR, ¹H NMR和元素分析确证.     

3-氯-4-二苄胺基-5-甲氧基-2(5H)-呋喃酮的合成与晶体结构

在THF溶液中合成了标题化合物3-氯-4-二苄胺基-5-甲氧基-2(5H)-呋喃酮,并用FT-IR、UV-Vis、1HNMR、13C NMR、MS、元素分析和X-射线衍射等进行了表征。结果表明此化合物属正交晶系,空间群为Pbca,晶胞参数为:a=15.891(16),b=11.126(11),c=19.778(19),α=β=γ=90°,V=3497(6)3,Z=8,Dc=1.306Mg/m3,μ=0.234 mm-1,F(000)=1440。在化合物的分子结构中,两个苯环几乎垂直于呋喃酮平面,且它们与呋喃酮平面的两面角分别为89.38°和88.19°。     

Poly (1,3-[2-methoxy-4-hydroxy-5-acetylphenylene] butylene) (HMAP-BG) as a polymeric ligand

Poly(1,3[2-methoxy-4-hydroxy-5-acetylphenylene]butylene) was prepared by Friedel-Craft polycondensation of 2-hydroxy, 4-methoxyacetophenone and 1,4-butane-diol in presence of poiyphosphoric acid catalyst. The polymer samples were characterized by IR spectra, TGA and their M_n determined by nonaqueous titration. Viscosity measurents in DMSO showed that solutions exhibited normal behaviour. Polymers were complexed with Cu(II), Ni(II), Mn(II), Co(II) and Zn(II) and characterized. Chelation and ion exchange properties were also studied by employing the batch equilibrium method.     

Microwave Synthesis and Crystal Structure of Bis {2- [（2,4-dichloro-phenylimino）- methyl]-4,6-diiodo-phenol}-copper（II）

Bis{2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol}-copper(II) (1) has been synthesized and its structure determined by X-ray diffraction. It crystallizes in the monoclinic system, space group P2 1 /n with a=14.7558(17), b=20.770(2), c=20.3260(19) , β=90.6110(10)°, V=6229.2(11) 3 and Z=8. The Cu atom is surrounded by two O atoms and two N atoms from two 2-[(2,4-dichloro-phenylimino)-methyl]-4,6-diiodo-phenol molecules to form a tetrahedral coordination environment. The complex is linked into a column by weak intermolecular interactions.     

Synthesis, characterization and thermal degradation of oligo-2-[(4-fluorophenyl) imino methylene] phenol and some of its oligomer-metal complexes

In this study, the oxidative polycondensation reaction conditions of 2-[(4-fluorophenyl) imino methylene] phenol (FPIMP) with air oxygen and NaOCl were studied in an aqueous alkaline medium between 60 and 90 °C. Synthesized oligo-2-[(4-fluorophenyl) imino methylene] phenol was characterized by ¹H-NMR, FT-IR, UV-Vis, size exclusion chromatography (SEC) and elemental analysis techniques. The yield of oligo-2-[(4-fluorophenyl) imino methylene] phenol (OFPIMP) was found to be 62.00% (for air O₂ oxidant) and 97.70% (for NaOCl oxidant) at the optimum reaction conditions. According to the SEC analysis, the number-average molecular weight (M_n), weight-average molecular weight (M_w) and polydispersity index (PDI) values of OFPIMP were found to be 1370 g mol⁻¹, 1979 g mol⁻¹ and 1.45, using NaOCl, 2105 g mol⁻¹, 2557 g mol⁻¹, and 1.22, using air O₂, respectively. During the oxidative polycondensation reaction, (2.88%) a part of -CHN group oxidized to carboxylic acid (-COOH). TG and TG-DTA analyses were shown to be more stable of oligo-2-[(4-fluorophenyl) imino methylene] phenol and its oligomer metal complexes than monomer against thermo-oxidative decomposition. The weight loss of OFPIMP was found to be 97.00% at 900 °C. The weight losses of OFPIMP-Co, OFPIMP-Ni OFPIMP-Cu oligomer-metal complex compounds were found to be 88.66%, 94.36% and 83.21%, respectively, at 1000 °C.