3-甲基犬尿喹啉酸衍生物的合成

报道了六个具有潜在生物活性 3 甲基犬尿喹啉酸衍生物的合成 .它们以取代苯胺和 3 甲基 2 酮丁二酸二乙酯为起始原料 ,经加成脱水 ,环化而得到 .其中三个新的含氟化合物的结构分别经IR ,1 HNMR ,MS ,元素分析等表征     

The effects of ring substituents in aniline on the reactivity of PANI with hydrogen tetrachloroaurate and the dispersion of gold nanoparticles

As expected from theoretical predictions, the polymerization of aniline was affected by the substituent group on the benzene ring. The rate of the polymerization varied as poly(2‐chloroaniline) (PANICl) < < poly(2‐methylaniline) (PANIMe) < polyaniline (PANI). While the rate of polymerization was determined largely by electronic effects of the substituent groups, the reactivity of the polymers was determined by the steric effects. The order of the rate of reaction of the polymers with AuCl₄⁻ was PANIMe < PANICl < < PANI. The amount of Au incorporated into the polymer matrix followed a similar trend. However, the size of the gold nanoparticles did not differ greatly. Gold nanoparticles dispersed on PANICl and PANIMe were more stable in acidic media than those on PANI. Copyright © 2015 John Wiley & Sons, Ltd.     

Room‐temperature Suzuki–Miyaura cross‐coupling reaction with α‐diimine Pd(II) catalysts

An α‐diimine Pd(II) complex containing chiral sec‐phenethyl groups, {bis[N,N′‐(4‐methyl‐2‐sec‐phenethylphenyl)imino]‐2,3‐butadiene}dichloropalladium (rac‐ C1 ), was synthesized and characterized. rac‐ C1 was applied as an efficient catalyst for the Suzuki–Miyaura cross‐coupling reaction between various aniline halides and arylboronic acid in PEG‐400–H₂O at room temperature. Among a series of aniline halides, rac‐ C1 did not catalyze the cross‐coupling of aniline chlorides and fluorides but efficiently catalyzed the cross‐coupling of aniline bromides and iodides with phenylboronic acid. The catalytic activity reduced slightly with increasing steric hindrance of the aniline bromides. The complexes {bis[N,N′‐(4‐fluoro‐2,6‐diphenylphenyl)imino]‐2,3‐butadiene}dichloropalladium and {bis[N,N′‐(4‐fluoro‐2,6‐diphenylphenyl)imino]acenaphthene}dichloropalladium were also found to be efficient catalysts for the reaction. Copyright © 2015 John Wiley & Sons, Ltd.     

Research on the direct amination of benzene to aniline by NiAlPO4–5 catalyst

A series of NiAlPO₄–5 molecular sieves have been hydrothermally synthesized and shown high and stable activity in the direct amination of benzene to aniline with hydroxylamine hydrochloride as aminating agent. The as‐synthesized and calcined samples were investigated with XRD, SEM, TG, BET, NH₃‐TPD and FT‐IR to explore the crystalline, coordination and location of the incorporated transition metal ions. The results indicated that nickel ions were incorporated into the framework of AlPO₄–5 and the as‐synthesized catalysts were highly crystalline, and possessed good thermal stability. Among them, Ni(0.3)AlPO₄–5 showed the highest catalytic activity for the direct amination of benzene with the highest aniline yield of 73.2% and 100.0% selectivity to aniline. After the catalyst was reused for 5 times, the activity remained little change.     

新显色剂2-(2-咪唑偶氮)-5-二乙氨基苯胺与钯显色反应的研究

研究了新显色剂2-2-(咪唑偶氮)-5-二乙氨基苯胺(IZAEA)与Pd2+显色反应的条件。试验结果表明,在pHL5. 0的HOAc-NaOAc介质中,试剂与Pd2+形成稳定的紫红色络合构,此络合物不被强酸分解,其它金属离子与试剂形成的有色络合构均被强酸分解。络合物的λmax为564nm,试剂的λmax为476nm,对比度△λ为88nm,Pd2+与试剂的络合比为l2,表观摩尔吸光系数为2．81×104L·mol-1·cm-1,Pdz+浓度在0～0．8mg·L-1范围内遵守比耳定律。所拟方法直接测定催化剂和分子筛中微量钯,结果满意。     

Vibrational Spectra of Benzylidene Aniline,O-Hydroxybenzylidene O-Hydroxyaniline and its Complexes with Cu(II) and NI(II) Metal Ions

Abstract

The FTIR and FT Raman spectra of benzylidene aniline, and o-hydroxybenzylidene o-hydroxyaniline compounds in the solid state in the wavenumber (1800-200 cm^?1) are recorded. An assignment for nearly all fundamentals are proposed. Comparison of the spectra of trans stilbene and benzylidene aniline reveals that v N-Ph stretch for the latter compound is situated at 1368 cm^?1 in the IR spectra with medium intensity. for o-hydroxybenzylidene o-hydroxyaniline, the stretching modes v N-Ph, and v C-Ph are observed at 1356 and 1226 cm^?1 respectively. the two v O-Ph are observed as intense bands in the IR spectra at 1245 and 1278 cm^?1, respectively. the FTIR spectra of the o-hydroxybenzylidene o-hydroxyaniline complexes with Cu(II) and Ni(II) metal ions are also recorded and assigned.     

Thermodynamics of polystyrene solutions. I. Interaction parameters and polymer order

The Maron theory was used to deduce from mostly osmotic pressure and light-scattering data the interaction parameters as a function of concentration, temperature, and polymer molecular weight for solutions of polystyrene in seven different solvents. These interaction parameters were then utilized to calculate the activity coefficients of the solvent in more concentrated solutions for comparison with experimental values deduced from vapor pressure measurements. When order was absent in the polymers (all cases but two), the agreement between calculated and observed activity coefficients was found to be very good. In the two cases where order was present, the activity coefficients observed in the concentrated solutions were higher than those calculated. These deviations were employed to find the degree of polymer order both in solution and in the original polymers.     

水溶性苯胺蓝光度法测定蛋白质

在pH1．0～2．3的酸性介质中,水溶性苯胺蓝与牛血清蛋白、人血清蛋白、卵白蛋白、α-糜蛋白酶作用形成结合产物时将导致溶液光吸收发生变化,在558nm褪色,在634nm附近吸光度增强,且吸光度差(△A)值均与蛋白浓度成正比,不同蛋白质分别在0～50mg／L或20～80mg／L范围内符合比耳定律。据此,建立了一种新的光度测定蛋白质的新方法。它用于人血清和尿液样品中总蛋白质的质量测定,回收率在95％～102％之间,结果满意。     

预处理条件对一步法合成吲哚用Ag/SiO2催化剂活性的影响

 以简单浸渍法制备的Ag/SiO2催化剂对苯胺和乙二醇一步法合成吲哚具有很高的催化活性. 研究了预处理条件对催化剂活性的影响. 结果表明,采用程序升温法将催化剂前体在500 ℃焙烧4 h,并在低于150 ℃时用H2-N2混合气(H2含量低于50%)原位还原得到的Ag/SiO2催化剂活性较高; TEM和XRD结果表明,预处理后催化剂表面银晶粒较小,结晶度较低.     

用于一步法高效合成吲哚的Cu/SiO2催化剂的研究

 采用等体积浸渍法制备了Cu/SiO2催化剂,并将其用于一步法合成吲哚反应. 结果表明,当Cu/SiO2催化剂中铜负载量为0.68 mmol/g,焙烧温度为600 ℃,并且在150 ℃下经50%H2-50%N2混合气还原后,其催化性能最佳,吲哚收率可高达88%; 当Cu/SiO2催化剂中金属铜的晶体达到一定结晶度时,其选择性很高,铜晶体的结晶度过高或过低都会导致副产物增多,吲哚选择性降低.