N-(取代苯氨基硫代甲酰基)邻苯二甲酰胺酸的合成

本文用四种硫脲衍生物和一种脲衍生物同邻苯二甲酸杆进行单酰化反应, 筛选了最适宜反应条件, 避免了环状副产物, 合成了N-(取代萃氨基硫代甲酰基)邻苯二甲酸。     

Nd（P_（507））_3－Al（i－Bu）_3催化马来酸酐与环氧丙烷开环交替共聚

本文研究了马来酸酐和环氧丙烷交替共聚，发现Ｎｄ（Ｐ_（５０７））_３－Ａｌ（ｉ－Ｂｕ）_３是马来酸酐（ＭＡｎ）和环氧丙烷（ＰＯ）交替共聚的良好催化剂，并用红外光谱，核磁共振谱研究了共聚物的结构。     

COORDINATION COPOLYMERIZATION OF STYRENE WITH MALEIC ANHYDRIDE BY RARE-EARTH COORDINATION CATALYSTS

The study on coordination copolymerization of styrene (S) with maleic anhydride (MA) by rare-earth coordination catalysts, NdL_3-Al(i-Bu)_3, has been successfully carried out for the first time. Some features, kinetic behavior, and mechanism of the SMA copolymerization by Nd(naph)_3-Al(i-Bu)_3 system are described and discussed. The copolymex of styrenemaleic anhydride prepared by the NdL_3-Al(i-Bu)_3 systems in benzene at 50℃ is an alternating-rich white powder having high number-average molecular weight of 6—8.5×10~5. The overall activation energy for the polymerization was found to be 10.5KJ/mol. The polymerization was not suppressed by addition of hydroquinone. The catalytic activity of various ligands in NdL_3 for the copolymerization decreases in the following order: Nd (naph)_3>Nd-(P_(507))_3～NdCl_3-6H_2O>Nd(P_(204))_3>Nd(acac)_3. 3H_2O. The experimental results are explained based on a mechanism to be the coordination-type copolymerization in terms of the participation of a monomer-monomer c     

马来酸酐与1，2－环己烷二羧酸二异丁酯的气液平衡

采用小沸点仪测定了马来酸酐和1,2－环己烷二羧酸二异丁酯二元系统在不同配料组成条件下的温度与压力数据，并通过内插法得到不同压力下的温度与配料组成的数据.进一步采用单纯形法优化NRTL方程参数，推算了平衡气液相组成，发现该二元系统具有最高压力恒沸点，且该恒沸点随压力的变化显著.当压力降低至20 kPa时, 由温度随气相组成的变化趋势知该恒沸点将趋于消失.     

Efficient, highly regioselective, and stereospecific conversion of glycidol systems into C2-O-acylated vicinal halohydrins

Glycidyl esters and ethers undergo a regioselective and stereospecific opening of the oxirane ring upon treatment in chloroform in the presence of pyridine with trimethylsilyl halide (TMSX, X = Cl, Br, or I) and a mixture of carboxylic acid (CA)-trifluoroacetic anhydride (TFAA), to produce the corresponding C2-O-acylated vicinal halohydrins in high yields.     

Controlled alternating copolymerization of St with MAh in the presence of DBTTC

The copolymerization of styrene (St) with maleic anhydride (MAh) performed at 22 °C in the presence of dibenzyl trithiocarbonate exhibits controlled nature evidenced by: narrow molecular weight distribution, controlled molecular weight and first-order polymerization kinetics. The composition analysis of the copolymers obtained by ¹³C NMR spectra shows the molar fraction of St in obtained copolymers is almost equal to 0.5 throughout the copolymerization. The sequence structure of the copolymer was obtained from DEPT experiments by recording the spectra at π/4 and 3π/4, and then combining them together, the results showed that the copolymers obtained possessed well-defined alternating structure. The experiment shows that charge-transfer-complex formed from St and MAh participates in both initiation and chain growth throughout the copolymerization.     

Carboxylic Acids from <Emphasis Type="Italic">Phyllanthus urinaria</Emphasis>

Five compounds, terephthalic acid mono-[2-(4-carboxy-phenoxycarbonyl)-vinyl] ester (1), (E)-3-(5′-hydroperoxy-2,2′-dihydroxy[1,1′-biphenyl]-4-yl)-2-propenoic acid (2), 3,4,5-trihydroxybenzoic acid (3), succinic acid (or butanedioic acid) (4), and 2,3,4,5,6-pentahydroxybenzoic acid (5), were isolated from Phyllanthus urinaria. The structures of these compounds were elucidated by means of spectral techniques including IR, MS, and 1D/2D NMR. 1 and 2 are new compounds.__________Published in Khimiya Prirodnykh Soedinenii, No. 1, pp. 14–17, January–February, 2005.     

一步法合成N-1,3-二羟基丙烷-2-基烷基乙酰胺

以5-氨基烷基-2,2-二甲基-1,3-二噁烷为起始原料, 乙酸酐为酰化剂, 一步法选择性地合成氨基二醇类氨基乙酰化产物N-1,3-二羟基丙烷-2-基烷基乙酰胺. 该方法操作简便, 收率高. 所合成的4个新化合物的结构均经FTIR, ¹H NMR, ¹³C NMR及HRMS确证. N-3-(1,3-二羟基丙烷-2-基)丙基乙酰胺(1a)作为关键的中间体, 可以用于HIV-1 Tat/ PCAF BRD抑制剂4的合成.     

SYNTHESIS OF MESOPOROUS POLY(STYRENE-co-MALEIC ANHYDRIDE)/SILICA HYBRID MATERIALS VIA A NONSURFACTANT-TEMPLATED SOL-GEL PROCESS*

Mesoporous poly (styrene-co-maleic anhydride)/silica hybrid materials have been prepared. The synthesis wasachieved by the HCl-catalyzed sol-gel reactions of tetraethyl orthosilicate (TEOS) and styrene-maleic anhydride copolymerin the presence of 3-aminopropyl triethoxysilane (APTES) as a coupling agent and citric acid as a nonsurfactant template orpore-forming agent, followed by ethanol extraction. Characterization results from nitrogen sorption isotherms and powder X-ray diffraction indicate that polymer-modified mesoporous materials with large specific surface areas (e.g. 900 m~2/g) andpore volumes (e.g. 0.6 cm~3/g) could be prepared. As the citric acid concentration is increased, the specific surface areas, porevolumes and pore diameters of the hybrid materials increase.     

马来酸酐与聚烯烃接枝产物的表征

综述了马来酸酐与聚烯烃接枝产物的多种表征手段，重点分析了纯化处理，化学滴定以及红外分析方法的表征原理，应用和改进方法。