Synthesis of 4-hydroxy- and 3-aryl-4-amino- 2-trifluoromethylpyridines

Schemes for synthesizing 3-acyl-4-amino(hydroxy)-2-trifluoromethylpyridines from 3-acyl 4-amino-5,5,5-trifluoro-3-penten-2-ones via their diphenylboron chelate complexes have been suggested.Translated fromlzvestiyn Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2715–2718, November, 1996,     

高固体分羟基丙烯酸树脂的合成

采用溶液聚合法合成了高固体分低粘度的羟基丙烯酸树脂(HAR),详细讨论了引发剂、链转移剂、反应温度、溶剂等对HAR粘度的影响。由HAR和六次甲基二异氰酸酯反应制备了性能优异的高固体分双组分丙烯酸聚氨酯涂料。     

2-(H-酸偶氮)-4,5-二硝基苯酚与钍的显色反应研究及其应用

研究了 2 (H 酸偶氮 ) 4 ,5二硝基苯酚 (HADNP)与钍的显色反应 ,在 pH 5 .5HOAc NaOAc缓冲介质中 ,溴化十六烷基吡啶 (CPB)存在下 ,HADNP与钍反应生成 2∶1稳定紫红色络合物 ,λmax=6 2 0nm ,ε =1.2 3× 10 5L·mol- 1·cm- 1。钍含量在 0～ 30 μg/2 5ml内符合比耳定律 ,方法用于环境水样品中钍含量的测定 ,结果满意。     

褪色光度法测定芬顿体系中产生的羟自由基

建立了检测Fenton反应产生羟自由基的新方法。在pH3．5条件下，经自由基与甲基紫发生反应使甲基紫褪色，在580nm处用分光光度计测定其△A值的变化，可间接测定羟自由基的生成量。通过对测定条件的研究，得到最佳实验条件。甲基紫光度法稳定性好，可作为一种简便的筛选羟自由基清除剂的方法。     

Synthesis of 1,3-Diketones by Reaction of α-Haloketones with Acyl Cyanides Promoted by Samarium Diiodide

α-Haloketones reacted with acyl cyanides to form 1,3-diketones in the presence of samarium diiodide. The reaction was assumed to proceed via a mechanism involving samarium enolates formed in situ from α-haloketones.     

Uncatalyzed,One-pot Synthesis of 3,3'-(Benzylene)bis(4-hydroxy-2H-chromen-2-one)Derivatives under Thermal Solvent-free Conditions

A series of 3,3′‐(benzylene)bis(4‐hydroxy‐2H‐chromen‐2‐one) derivatives have been synthesized from condensation reactions of 4‐hydroxycoumarin with benzaldehydes under thermal solvent‐free conditions. This environmentally friendly synthesis is uncatalyzed and affords the desired products in excellent yields.     

4‐Hydroxy‐3‐carboxycoumarin as an efficient building block for new ruthenium(II) complexes: synthesis,characterization, antibacterial,antioxidant and anti‐inflammatory activities

A new 4‐hydroxy‐3‐carboxycoumarin ligand and its ruthenium(II) complexes ( 1 – 5 ) have been synthesized, characterized and screened for their in vitro antibacterial activity against a range of Gram‐positive and Gram‐negative bacteria. In addition, compounds 1 – 5 were investigated for antioxidant activities using superoxide radical, 2,2‐diphenyl‐1‐picrylhydrazyl radical and hydroxyl radical scavenging assays, in which most of them displayed significant antioxidant activities. Furthermore, compounds 1 – 5 were evaluated for anti‐inflammatory activity using indirect haemolytic and lipoxygenase inhibition assays and revealed good activity. The new complexes were characterized using spectroscopic methods in addition to elemental analysis.     

Practical Preparation of β‐Amino‐α‐Hydroxy Diesters: Key Intermediates for 1,4‐Oxazin‐2‐Ones

In the presence of a catalytic amount of amino acid hydrochloride, trans‐β‐phenylglycidic ester undergoes ring opening with high stereo‐ and regioselectivity when treated with glycine esters. Alkylation of the resulting β‐amino‐α‐hydroxy diesters with benzyl bromide, followed by cyclization to furnish the expected 1,4‐oxazin‐2‐ones, is also described.     

A new metabolite of nodakenetin by rat liver microsomes and its quantification by RP‐HPLC method

The biotransformation of nodakenetin (NANI) by rat liver microsomes in vitro was investigated. Two major polar metabolites were produced by liver microsomes from phenobarbital‐pretreated rats and detected by reversed‐phase high‐performance liquid chromatography (RP‐HPLC) analysis. The chemical structures of two metabolites were firmly identified as 3′(R)‐hydroxy‐nodakenetin‐3′‐ol and 3′(S)‐hydroxy‐nodakenetin‐3′‐ol, respectively, on the basis of their ¹H‐NMR, MS and optical rotation analysis. The latter was a new compound. A sensitive, selective and simple RP‐HPLC method has been developed for the simultaneous determination of NANI and its two major metabolites in rat liver microsomes. Chromatographic conditions comprise a C₁₈ column, a mobile phase with MeOH‐H₂O (40 : 60, v/v), a total run time of 40 min, and ultraviolet absorbance detection at 330 nm. In the rat heat‐inactivated liver microsomal supernatant, the lower limits of detection and quantification of metabolite I, metabolite II and NANI were 5.0, 2.0, 10.0 ng/mL and 20.0, 5.0, 50.0 ng/mL, respectively, and their calibration curves were linear over the concentration range 50–400, 20–120 and 150–24000 ng/mL, respectively. The results provided a firm basis for further evaluating the pharmacokinetics and clinical efficacy of NANI. Copyright © 2009 John Wiley & Sons, Ltd.     

Tandem Ring Opening and Oximation of Ethyl 3‐Aroyl‐1‐cyano‐4‐hydroxy‐2,4,6‐triarylcyclohexanecarboxylate by Hydroxylamine

The reaction of hydroxylamine hydrochloride with ethyl 3‐aroyl‐1‐cyano‐4‐hydroxy‐2,4,6‐triarylcyclohexanecarboxylate has led to the formation of ethyl 2‐[amino(hydroxyimino)methyl]‐3‐aryl‐5‐(hydroxyimino)‐5‐arylpentanoate via a tandem ring opening and oximation process. The structures of the products are confirmed by NMR and X‐ray techniques, and the conformational features of the product arrived at are compared with a molecular dynamics simulation study.