cis,trans-4-戊基环己基甲酸的合成及异构体转位

采用Ni5249P为催化剂，在水相碱性条件下，反应温度为175℃，反应压力为9MPa，加氢合成4-戊基环己基甲酸[m（civ）：m（trans-）=75：253。在200-220℃进行异构体转位，可以使4-戊基环己基甲酸产物中m（cir）：m（trans-）=2：98，trans-4-戊基环己基甲酸收率为95％。

4-(trans-4”’-n-烷基环己烷甲氧基)-4'-氰基联苯的合成

从trans－4－n-烷基环己基甲醇和4-溴-4’-羟基联苯出发经磺酸酯化、醚化、氰代合成了三种4－（trans-4”－n-烷基环己烷甲氧基）－4’-氰基联苯液晶化合物，经IR、MS、元素分析确证了化学结构．

Synthesis and Crystal Structure of Trans-4-[(5-(2,4-Dichlorophenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one

The title compound trans-4-[（5-（2,4-dichlorophenoxy）-3-methyl- 1-phenyl-1H-pyrazol-4-yl）methyleneamino]- 1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 （C28H23Cl2N5O2, Mr = 532.41） has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1- with a = 8.9438（4）, b = 11.6065（5）, c = 14.2215（6）A, α = 112.566（1）, β = 92.324（2）, γ = 102.91（1）°, V= 1315.65（10） A^3, Z = 2, Dc = 1.344 g/cm^3,μ（MoKa） = 0.282 mm^-1, λ = 0.71073 A, F（000） = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra- and intermolecular C（ 12）-H（12）…O（1） and C（28）-H（28）...O（1）# 1 hydrogen bonds were observed in the title compound.

Enantioselective esterification of(R,S)-2-(4-methylphenyl)propionic acid via Novozym 435:Optimization and application

This paper reports on the resolution of(R,S)-2-(4-methylphenyl)propionic acid(MPPA)enantiomers by enzymatic esterification in organic solvent.Novozym 435(CALB)has the best catalytic performance compared with other lipases.Of the alcohols screened,n-hexanol is the best acyl acceptor and gives the highest enzyme activity and enantioselectivity in n-hexane.Response surface methodology(RSM)was used to evaluate the influence of the factors,such as temperature,enzyme amount,substrate concentration and reaction time on the substrate conversion(c)and enantiomeric excess(ee).The correlation coefficient R2 for enantiomeric excess and the conversion are 0.9827 and 0.9910,respectively,indicating that can accurately predict the experimental results.By simulation and optimization,the optimal conditions were obtained,involving 600 mmol·L^-1 MPPA concentration(0.60 mmol),850 mmol·L^-1 hexanol concentration(0.85 mmol),58 mg enzyme amount,75℃temperature and 4.5 h reaction time,respectively.Under the optimized conditions,the experimental values of conversion and enantiomeric excess were 89.34%and 97.84%,respectively,which are in good agreement with the model predictions.

Synthesis of New Multibranch Chromophores with Strong Light-emitting in Solution and in PMMA Film

Three new chromophores with triphenylamine as molecular focal point bearing one, two, or three 4-(n-butyloxystyryl) group(s) at the periphery respectively, (named as T1, T2, and T3) have been synthesized and characterized. It is interesting to find that the fluorescence quantum yield increases from T1 (0.489), to T3 (0.535), and to T2 (0.628) in cyclohexane, meanwhile the lifetime for T3 is shorter than T1 and T2, which is an important characteristic for applications in light emitting diode. Also PMMA (polymethyl methacrylate) film doped with T3 gives stronger fluorescence than T1, and T2. Cyclic voltammetry showed that T3 exhibited lowest oxidation potential of 0.52 V vs SCE, suggesting its better hole-transport property.

Low and Wide Phase Transition Temperature Dimesogenic Compounds Consisting of a Cholesteryl and 4-（trans-4-n-Alkylcyclohexyl）phenoxy Mesogens

Unsymmetrical dimesogenic compounds with cholesteryl and 4-（trans-4-n-alkylcyclohexyl）phenoxy parts were synthesized by condensation of cholester-3-yl 6-bromohexanoate with appropriate 4-（trans-4-n-alkylcyclohexyl）- phenols. Structures and thermal phase behaviour of these dimesogenic compounds have been confirmed by IR, IH NMR, elemental analysis, DSC, polarity microscopy and XRD measurements. Their thermal phase behaviour was significantly different with that of other cholesterol-based dimesogens while they exhibited low and wide phase transition temperature.

Synthesis and anti-HIV activities of phorbol derivatives

In this study,37 derivatives of phorbol esters were synthesized and their anti-HIV-1 activities evaluated,building upon our previous synthesis of 51 phorbol derivatives.12-Para-electron-acceptor-trans-cinnamoyl-13-decanoyl phorbol derivatives stood out,demonstrating remarkable anti-HIV-1 activities and inhibitory effects on syncytia formation.These derivatives exhibited a higher safety index compared with the positive control drug.Among them,12-(trans-4-fluorocinnamoyl)-13-decanoyl phorbol,designated as compound 3c,exhibited the most potent anti-HIV-1 activity(EC_(50)2.9 nmol·L^(−1),CC50/EC_(50)11117.24)and significantly inhibited the formation of syncytium(EC_(50)7.0 nmol·L^(−1),CC50/EC_(50)4891.43).Moreover,compound 3c is hypothesized to act both as an HIV-1 entry inhibitor and as an HIV-1 reverse transcriptase inhibitor.Isothermal titration calorimetry and molecular docking studies indicated that compound 3c may also function as a natural activator of protein kinase C(PKC).Therefore,compound 3c emerges as a potential candidate for developing new anti-HIV drugs.

HPLC同时测定安息香中3种化学成分的含量

目的:建立HPLC同时测定安息香中香草醛、松柏醛和trans-[四氢-2-(4-羟基-3-甲氧基苯基)-5-氧代呋喃-3-基]甲基苯甲酸酯含量的方法。方法:采用Phenomenex Luna C18(2)色谱柱(4.6 mm×250 mm,5μm),以甲醇-水为流动相,在1.0 m L·min-1的流速下,对样品进行梯度洗脱,并在280 nm波长处测定这3种化学成分的含量。结果:3种成分均能达到基线分离,且线性关系良好,加样回收率分别为99.51%,101.25%,100.71%。结论:该方法灵敏、准确、具有良好的稳定性和重复性,可用于同时测定安息香中这3种化学成分的含量,为安息香的质量控制研究提供一定参考。