Synthesis and Crystal Structure of N-phenyl-N-[(o-nitrophenylacetyl)oxy]benzamide

The compound N-phenyl-N-[（o-nitrophenylacetyl）oxy]benzamide （C21HI6N2Os, Mr = 376） has been synthesized by the reaction of N-hydroxy-N-phenylbenzamide with 2-（2-nitro- phenyl）acetyl chloride in dichlorom-ethane and its structure Was characterized by 1H NMR, 13C NMR, IR, H RMS（ESI） and single-crystal X-ray diffraction. The crystal of the title compound belongs to monoclinic, space group C2/c with a = 32.30（2）, b = 8.400（5）, c = 15.099（9） A, fl = 114.256（10）°, V = 3735（4） A3, Z = 8, D, = 1.339 g/cm3, F（000） = 1568, p = 0.097 mm-1, the final R = 0.0506 and wR = 0.1176 for 2318 observed reflections （1 〉 2a（/））. The title molecule contains three branched chains with its center placed at the midpoint of N. The phenyl ring （C（1）＇-C（6）） makes a dihedral angle of 70.3（1）° with the phenyl ring （C（10）-C（15）） of benzoyl group, and 14.3（1）° with the phenyl ring （C（16） - C（21））, Hydrogen bonds C（5）-H（5）...O（1） and C（12）-H（12）...O（3） together with it-Jr stacking interactions contribute to the stability of the structure.

苯甲酰胺（Benzamide）对大麦辐射损伤的影响

本试验以苯甲酰胺和６０Ｃｏ—γ射线复合处理大麦种子，研究了其诱变效果。结果表明：苯甲酰胺没有诱变作用。辐射和苯甲酰胺复合处理，对大麦的出苗率、成株率、结实率、株高及苗高、Ｍ１根尖细胞染色体和花粉母细胞染色体畸变均有明显的影响，即苯甲酰胺加重了Ｍ１的损伤。同时还表明，在较低的照射剂量下，苯甲酰胺的修复抑制效果较好。本试验修复抑制效果最佳处理为２２０Ｇｙ＋１０ｍｍｏｌ／Ｌ。

苯甲酰胺(Benzamide)对大麦辐射损伤修复抑制及遗传效应的研究

本试验以大麦“吉农８７－９号”风干种子为材料，用不同剂量＾６０Ｃｏγ－射线处理后，再用苯甲酰胺（浓度为０、５、１０ｍＮ）处理，研究其诱变效应。结果表明：苯甲酰胺无诱变作用，但与γ－射线复合处理诱变效应优于γ－射线单因子处理。苯甲酰胺加重了Ｍ１辐射损伤，提高了Ｍ２突变频率。因此，在诱变育种中苯甲酰胺可作为有效的修复抑制剂加以利用。在较低的照射剂量下，苯甲酰胺修复抑制效果较好。

Synthesis, Crystal Structure and Antitumor Activity of N-[5-(Benzylthio)-1,3,4-thiadiazol-2-yl]-4-chlorobenzamide

The title compound N-[5-（benzylthio）-1,3,4-thiadiazol-2-yl]-4-chlorobenzamide（C（16）H（12）ClN3OS2, Mr = 361.86） was designed and synthesized as anticancer agent, and its crystal structure was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P1 with a = 5.7417（10）, b = 9.8057（17）, c = 14.330（3） A, a = 91.987（3）, b = 97.154（3）, γ = 93.402（3）°, V = 798.4（2） A3, Z = 2, Dc = 1.505 g/cm^3, μ = 0.507 mm-1） F（000） = 372, the final R = 0.0481 and wR = 0.1290 for 2064 observed reflections with I 〉 2s（I）. In the crystal packing, the molecules form stacks by a three-dimensional framework, which results from intermolecular N（1）-H（1）···N（2） and C（5）-H（5）···N（3） hydrogen bonds together with π-π stacking interactions between the thiadiazole and chlorobenzene rings. The title compound was found to exhibit more potent in vitro antitumor activities against the four tested cancer cell lines than sorafenib.

Synthesis and Bacteriostatic Activity and Antifouling Capability of Benzamide Derivatives Containing Capsaicin

Five benzamide deriatives containing capsaicin were synthesized which have similar structures to capsaicin. Their yield was high. The monomers synthesized were characterized by IR, 1H NMR and MS spectroscopy. Cha-racterization data are in agreement with the proposed structures of the products. These five compounds exhibit bacterial inhibition and N-[4-hydroxy-2-methyl-5-（methylthio）benzyl]benzamide（HMMBBA）, for instance, shows that the minimal inhibitory concentrations（MIC） of HMMBBA are 0.125 and 0.25 mg/mL on Staphyloccocus aureus and Escherichia coli, respectively. A static test site was set up in the eighth harbor to investigate the antifouling effectiveness of the five new antifoulants. Five-month exposure experiments were performed on sets of panels coated with each of antifouling coatings, and the results were compared to that of the test panel without antifouling coating. Test boards with antifouling coating were covered with just a macroscopic fouling organism such as Balanus. The results of the present paper demonstrate that new antifoulants represent an alternative to the biocidal antifouling paint.

Crystal and Molecular Structure of Bis-N,N’(dithiodi-2,1-phennylene)benzamide

The crystal structure of the title compound ((C 6H 5CONC 6H 4S) 2, M r =229) has been determined by X ray diffraction analysis. The crystal belongs to triclinic space group P 1 with cell parameters: a=7.957(4), b=11.570(7), c=12 335(6), α=76.68(4), β=81.48(4), γ=87.26(4)°, V=1092.9 3, Z=2, D c =1 39g/cm 3, F(000)=476, μ (Mo Kα )=2.7mm -1 . The final R factor is 0.0373 for 3764 observed reflections. The result of X ray diffraction analysis indicates that all of these single bond lengths are obviously shorter than that of standard single bond. Those atoms might take part in a conjugate system. The electrons for sp 3 hybridized S(1) and S(2) move toward two sides and the densities of electronic cloud among them are reduced and can be easily broken. The obtained results can explain the reaction mechanism of the title compound.

Synthesis, Characterization and X-ray Crystal Structure of 4-Fluoro-N-(2-methyl-5-((2-(p-tolyloxy)acetamido)- methyl)pyrimidin-4-yl)benzamide

A new crystal of 4-fluoro-N-（2-methyl-5-（（2-（p-tolyloxy）acetamido）methyl）pyrimi- din-4-yl）benzamide has been prepared at room temperature and characterized by 1H NMR, 13C- NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic, space group P21 /c with a = 17.226（5）, b = 13.934（4）, c = 17.262（5）, μ= 92.180（5）°, V = 4140（2） ？3, Dc = 1.311 g/cm3, Z = 8, F（000） = 1712 and ？？= 0.095 mm-1. The molecular packing in the crystal is the result of N-H…ydrogen bonds.

Evaluation of Benzamide Derivatives as New Influenza A Nucleoprotein Inhibitors

Virus nucleoprotein (NP) is an emerging target for drug development for Influenza. We designed benzamide derivatives as new inhibitors of NP that demonstrate good potency in blocking influenza A. Screening revealed that compound 39 was the most potent molecule in the series, exhibiting IC50 values of 0.46 and 0.27 μM in blocking the replication of H3N2 (A/HK/8/68) and (A/WSN/33) influenza A viral strains. The observed inhibition of viral replication correlated well with cytopathic protection. Furthermore, based on computational analysis and fluorescence microscopy, it was determined that compound 39 inhibited nuclear accumulation by targeting influenza A viral nucleoproteins. Finally, the rodent pharmacokinetic profile of compound 32 displayed half-life of greater than 4 hours and bioavailability greater than 20%, suggesting this class of molecules had drug-like properties.

Synthesis and Crystal Structure of 3,5-Dichloro-N-(2-methoxyphenyl)benzamide

The title compound was synthesized by the direct reaction of 3,5-dichlorobenzoic acid with 2-methoxyaniline in the presence of DCC and HOBT. The structure was supported by the spectroscopic data and unambiguously confirmed by the single-crystal X-ray diffraction studies. It crystallizes from a methanol solution in the monoclinic space group P21/c with unit cell dimensions of a = 4.9369（16）, b = 13.351（5）, c = 20.168（7） A, β = 96.755（8）°, V= 1320.1（8） A^3 and Z=4.

Synthesis and Crystal Structure of 4-Chloro-N-(2-(2-nitrophenyl)acetoxy)-N-(m-tolyl)benzamide

The new title compound 4-chloro-N-（2-（2-nitrophenyl）acetoxy）-N-（m-tolyl）benza- mide （C：2HI7C1N2Os, Mr = 424.82） has been synthesized via the reaction of 4-chloro-N-hydroxy-N- （m-tolyl）benzamide with 2-（2-nitrophenyl）acetyl chloride. The structure of the product was confirmed by 1H NMR, 13C NMR, IR, HRMS （ESI） and single-crystal X-ray diffraction. The title compound crystallizes in the monoclinic system, space group P21/c with a = 13.0269（10）, b =6.7251（6）, c = 23.9313（16） A, β = 99.931（6）°, V = 2065.1（3） A3, Z = 4, Dc = 1.366 g/cm3, F（000） = 880,μ = 0.221 mm-1, the final R = 0.0600 and wR = 0.1754 for 1981 observed reflections （I〉 20（/））. X-ray analysis indicates that the chloro-phenyl ring （C（10）℃（15）） and the methyl-substituted benzene ring （C（16）℃（21）） are not coplanar with the nitro-substituted benzene ring （C（1）--C（6））, with the dihedral angle to be 70.78° and 63.72°, respectively. Hydrogen bonds C（2）-H（2）...O（2） and C（7）-H（7B）...O（5） are observed.

Rate Enhancements in the Acetylation and Benzoylation of Certain Aromatic Compounds with Vilsmeier-Haack Reagents Using Acetamide, Benzamide and Oxychlorides under Non-Conventional Conditions

Acetylation and benzoylation reactions of certain aromatic aldehydes, ketones with Vilsmeier-Haack Re- agents using Acetamide and Oxychloride (SOCl2 or POCl3) under conventional (thermal) and non conven- tional [microwave irradiated (MIR), ultrasonic assisted and solvent free mortar pestle (grinding)] conditions. Reactions afforded good to excellent yields of products with both the VH reagents, reaction times were fairly less in the case of [amide/POCl3] than those of [amide/SOCl2] reagent. Reactions are dramatically acceler- ated in under sonicated and microwave irradiations with a trend: MIR (few seconds) >> Sonication (minutes) > Grinding (min) >> thermal (several hrs).

Crystal and Molecular Structure of N-[2-(6-Methoxy-2-oxo-2H-Chromen-4-yl-Benzofuran-3-yl]- Benzamide

The crystal structure of the potential active N-[2-(6-Methoxy-2-oxo-2H-chromen-4-yl)-benzofuran-3-yl]-benzamide (C25H17NO5) (I) has been determined from single crystal X-ray diffraction data. The title compound crystallizes in the monoclinic space group P 21/n, with a = 12.0551(11), b = 9.7853(8), c = 16.6517(16) , β = 90.092(4)o, V = 1964.28(3) 3, Dcalc = 1.391 Mg/m3, Z = 4. In the structure, intermolecular H-bonds lead to the formation of a centrosymmetric dimer of the molecule. There is an intramolecular C7—H7…N1 hydrogen bond forming a closed seven membered ring. There are also intramolecular π-π interactions presented between the 3,6-Dihydro-2H-pyran ring of the chromen moiety [Cg2…Cg2 distance = 3.5812(13) ]. The packing structure is stabilized by these C—H…N, N—H…O hydrogen bonds, C—H… π and π…π interactions.

BANDED TEXTURE FORMATION IN NEMATIC SOLUTION OF POLY (1,4-BENZAMIDE) IN SULFURIC ACID

The banded texture in films prepared from nematic poly (1,4-benzamide) (PBA)/H_2SO_4 solution by shearing and without shearing has been studied by using microscopy techniques. The kinetic parameters of banded texture formation γ_c and τ_b were measured for nematic solution of PBA by using parallel-plate shearing apparatus. The banded texture was also observed in randomly packed domains for nematic solution of PBA on standing without shearing. The properties of banded texture show no difference between the two samples with or without shearing.

含喹唑啉结构的苯甲酰胺类衍生物合成及抗菌活性

以溴代邻氨基苯甲酸为原料,运用活性结构拼接法,设计合成了17个新型的含喹唑啉结构的苯甲酰胺类衍生物(Ⅳ_(a)~Ⅳ_(q))。通过~1H NMR、^(13)C NMR、HRMS和元素分析对化合物进行了结构确认,并以叶枯唑为阳性对照药物,分别在50μg·mL^(-1)、100μg·mL^(-1)浓度下,测试了所有产物对3种常见植物细菌(水稻白叶枯细菌(Xoo)、猕猴桃溃疡病菌(Psa)、柑橘溃疡病菌(Xac))的体外抗菌活性。由于化合物Ⅳ_(d)在两个浓度时对3种细菌抑菌率普遍高于其他16个化合物,且对水稻白叶枯细菌(Xoo)的抑菌率高达100%,明显高于化合物Ⅳ_(d)对另外2种细菌的抑菌率,因此对化合物Ⅳ_(d)进行了抗水稻白叶枯细菌(Xoo)作用机制研究。结果表明:大部分目标化合物对三种病菌都具有一定的抑制活性,其中化合物Ⅳ_(d)表现出较好的抑菌作用。在菌体浓度为10~8CFU/mL,化合物Ⅳ_(d)对Xoo的最低抑菌浓度(MIC)为100μg·mL^(-1),化合物Ⅳ_(d)可通过改变Xoo细胞膜的通透性,在一定程度上破坏菌体的细胞膜,使病原菌细胞内的蛋白质发生泄露,并且化合物Ⅳ_(d)浓度越高,对细胞膜通透性的影响越大;当目标化合物Ⅳ_(d)浓度达到2MIC时,可显著降低3种关键菌体胞内酶活性,从而影响Xoo菌体正常的能量代谢,起到抑菌作用。

Synthesis,Characterization and X-ray Crystal Structure of 2-Methylpropan-2-aminium Methyl ((4-Fluorobenzamido)(4-fluorophenyl)methyl) phosphonate·H_2O

A new crystal of 2-methylpropan-2-aminium methyl （（4-fluorobenzamido）（4- fluorophenyl）methyl）phosphonate has been prepared at room temperature and characterized by ZH- NMR, 13C NMR, IR, MS, elemental analysis and X-ray single-crystal determination. The compound crystallizes in monoclinic space, group C2/c with a = 20.719（2）, b = 11.8559（13）, c = 18.176（2） A,β = 94.434（2）°, V= 4451.4（9） A3, Dc = 1.317 Mg/m3, Z= 8, F（000） = 1864 and μ= 0.174 mm-1. The crystal packing is stabilized by intermolecular N-H……O and O-H……O hydrogen bonds, as well as by weak π-π stacking interactions.

抗耐药铜绿假单胞菌DK2增敏剂的结构优化与活性评价

目的发现有效增敏多粘菌素B抗耐药铜绿假单胞菌DK2,并且具有良好安全性和水溶性的化合物。方法将本课题组前期所发现的先导化合物B4进行苯甲酰胺类化合物的设计与合成,并且通过微量肉汤稀释法测试目标化合物对铜绿假单胞菌DK2的体外增敏活性,CCK8测试优选目标化合物HEK-293细胞毒性及HPLC法测试优选目标化合物的水溶性。结果合成了19个目标化合物并进行了结构确证及DK2菌株体外增敏活性测定,其中,目标化合物15a和24a在浓度为32μg·mL^(-1)时将多粘菌素B增敏到浓度为1μg·mL^(-1),并且安全性明显优于B4。此外,24a水溶性优于15a,但未优于B4。结论通过结构改造,得到优选目标化合物24a,为后续开发增敏多粘菌素B抗耐药铜绿假单胞菌DK2的候选药物提供了良好的结构基础。

3,4,5-三(甲氧基乙氧基乙氧基)-N-炔丙基苯甲酰胺的合成及温度响应性能研究

通过3,4,5-三(甲氧基乙氧基乙氧基)苯甲酸与炔丙基胺的反应,合成了3,4,5-三(甲氧基乙氧基乙氧基)-N-炔丙基苯甲酰胺,用1H NMR谱和ESI-MS确定了产物结构;并研究了三种溶剂(N,N-二甲基甲酰胺、四氢呋喃和二氯甲烷)对目标产物产率的影响;用紫外-可见分光光度计研究了产物的温度响应性能。结果表明,采用二氯甲烷为溶剂时,产物的产率最高,为81.36%;产物具有温度响应性,其低临界溶液温度(LCST)随产物浓度的增加而降低。

钴催化氘代甲氧基化苯甲酰胺衍生物的合成研究

由于C-D键独特的稳定性和标记作用,在化合物中引入氘对于候选药物的合成以及反应机理的研究具有重要意义。芳基醚是一种在药物、溶剂和聚合物前体等方面具有应用前景与价值的化合物,广泛存在于药物中间体和农业生产中。本文根据C-D键和芳基醚类化合物的双重优势,以氘代甲醇为氘源,开发了一种钴(II)/水杨醛配体组成的催化体系,在氧化条件下高效合成了氘代甲氧基化芳烃化合物,该方法无需使用酸碱添加剂,反应条件温和,具有良好的官能团相容性和氘掺入量,各种不同取代的苯甲酰胺衍生物产率中等至良好。

高效液相色谱-串联质谱法同时测定盐酸拉贝洛尔中三种杂质

建立高效液相色谱-串联质谱法同时测定盐酸拉贝洛尔中2-羟基-5-[1-羟基-2-[(1-甲基-3-苯丙基)氨基]乙基]苯甲酸、2-羟基-5-[1-羟基-2-[(1-甲基-3-苯丙基)氨基]乙基]苯甲酸甲酯和2-羟基-5-(2-(4-苯基丁-2-氨基)乙酰)苯甲酰胺的含量。采用Agilent Eclipse XDB-C18柱(250 mm×4.6 mm,5μm)为分离柱,以0.1%(质量分数)的乙酸溶液为流动相A,乙腈-0.1%的乙酸溶液(体积比为1∶1)为流动相B,流量为1.5 mL/min,梯度洗脱,柱温为40℃,进样体积为10μL,离子源为大气压化学电离源,采用多反应监测模式。三种杂质的质量浓度分别在1.0160~203.20、1.0320~206.40、1.0370~207.40 ng/mL范围内与色谱峰面积线性相关,相关系数均大于0.999,3种化合物的检出限均为0.03 ng/mL,定量限均为0.10 ng/mL。样品平均回收率分别为95.3%、92.4%、91.9%,测定结果的相对标准偏差分别为1.44%、1.46%、1.11%(n=9)。该方法可用于同时测定盐酸拉贝洛尔中3种杂质,有效地监测盐酸拉贝洛尔的质量。