γ-氨基丁酰胺的合成研究

γ-氨基丁酰胺在食品,医药等领域有着重要作用,但是现有合成路线繁琐、反应条件苛刻、最终产率较低.本文设计以γ-氨基丁酸为原料,经过酰化、氨解作用合成γ-氨基丁酰胺.同时考察了不同的反应条件对产品收率的影响.工艺成熟,适宜工业化生产.     

交流示波极谱法测定工业污水中的微量汞

本文提出了用交流示波极谱法测定工业废水中的微量汞。在pH=6的HAc-NaAc缓冲液中,有Br-存在时,Hg2 在金电极上有敏锐的切口,可用于指示终点。方法简便、快速、准确,终点清晰、直观,切口敏锐,不受颜色和沉淀的影响,用于废水中的微量汞的测定,结果满意。     

工业废水中微量苯酚的交流示波极谱滴定

工业废水中微量污染物苯酚用交流示波极谱滴定可简单而快速地测定。准确分取部分过滤后的试样在氯化钾底液中以苯胺作指示剂,在不断搅拌下用0.020 00 mol.L-1氢氧化钾标准溶液滴定,用汞膜电极作指示电极,银汞电极为参比电极。苯胺的示波极谱图上出现切口时即为滴定终点。根据氢氧化钾标准溶液滴定的体积计算试样中苯酚的含量。此滴定至终点的溶液的pH值经预先试验测定为11.27,而6 g.L-1苯胺溶液1 mL在氯化钾底液中当出现切口时的pH值为11.3。苯胺在此方法中的作用为指示剂,以其示波极谱图上出现切口指示滴定终点。此方法应用于废水样品分析,回收率在97.3%~104.0%之间。     

Synthesis,Crystal Structure,Antitumor Activities and Docking Study of 1-(2-(1H-Indol-3-yl)ethyl)-3-(2-methoxyphenyl)urea

The title compound,1-(2-(1 H-indol-3-yl)ethyl)-3-(2-methoxyphenyl)urea(C_(18)H_(19)N_3O_2,M_r = 309.36) has been synthesized,and its structure was characterized by ~1H-NMR,~(13)C-NMR,ESI-MS and single-crystal X-ray diffraction.It crystallizes in the monoclinic space group P2_1/c with a = 16.2774(15),b = 11.1082(10),c = 9.0819(3) ?,β = 103.09(9)°,V = 1599.5(3) ?~3,Z = 4,T = 293(2) K,μ(MoKα) = 0.086 mm~(-1),D_c = 1.285 g/cm~3,F(000) = 656 and GOOF = 0.981.5973 reflections were measured(7.04≤2θ≤52.04°),and 3143 were unique(Rint= 0.0393,Rsigma = 0.0546) and used in all calculations.The final R = 0.0756(I 2σ(I)) and w R = 0.1976(all data).The antitumor activity of the title compound was analyzed by MTT assay.Meanwhile,to rationalize its potencies in the CDK4 target,the title compound was docked into CDK4 protein and the interactions with the active site residues were analyzed.     

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)benzamide(C22H17ClN2O5, 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, 13 C 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) , β = 99.931(6)o, V = 2065.1(3) 3, 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 2σ(I)). X-ray analysis indicates that the chloro-phenyl ring(C(10)~C(15)) and the methyl-substituted benzene ring(C(16)~C(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.     

Synthesis,Crystal Structure and Antitumor Activities of Ethyl(R)-2-(Biphenyl-4-carbonyl)-2,3,4,9-tetrahydro-1H-pyrido[3,4-b]indole-1-carboxylate

The title compound,ethyl(R)-2-(biphenyl-4-carbonyl)-2,3,4,9-tetrahydro-1H-pyri do-[3,4-b]indole-1-carboxylate(C_(27)H_(24)N_2O_3) has been synthesized,and its structure was charac-terized by ~1H-NMR,~(13)C-NMR,ESI-MS and single-crystal X-ray diffraction.It crystallizes in the orthorhombic system,space group Pbca with a = 16.9950(8),b = 9.5445(4),c = 28.3188(3) ?,V = 4593.6(3) ?~3,Z = 8,T = 294.64(10) K,μ(MoKα) = 0.08 mm~(-1),Dc = 1.228 g/cm~3,F(000) = 1792 and GOOF = 1.036.11836 reflections were measured(7.04≤2θ≤52.04°),and 4506 were unique(R_(int)= 0.0393,R_(sigma )= 0.0546) and used in all calculations.The final R = 0.0576(I 2σ(I)) and wR = 0.1563(all data).The preliminary biological tests show that the title compound has a good antitumor activity against Hela in vitro with the IC_(50) value of 4.71 μmol/L.     

Synthesis,Crystal Structure and Antitumor Activities of N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline

The title compound, N-(2-(1H-indol-3-yl)ethyl)-2-nitroaniline(C16H15N3O2, Mr = 281.31), has been synthesized by the multicomponent reaction of milder Ullmann, and its structure was characterized by 1H NMR, 13 C NMR, IR, H RMS(ESI) and single-crystal X-ray diffraction. It crystallizes in monoclinic, space group I2/c with a = 15.0212(10), b = 9.4911(6), c = 20.3075(13) A, β = 100.776(7)o, V = 2844.1(3)A3, Z = 8, Dc = 1.314 g/cm3, F(000) = 1184.0, μ = 0.089 mm-1, the final R = 0.0574 and w R = 0.1688 for 1701 observed reflections(I 2σ(I)). X-ray analysis indicates three major N(2)–H(2)···O(2), C(13)–H(13)···O(2), N(2)–H(2)···N(3) hydrogen bonds and π-π stacking interactions in the crystal structure. The preliminary biological test shows that the title compound has a good antitumor activity against A549 in vitro with the IC50 value of 35 μmol/L.