Asymmetric synthesis of cis-5-tert-butylproline with metal carbenoid NH insertion

The highly stereoselective intramolecular metal carbenoid insertion reaction of sulfinimine-derived delta-amino alpha-diazoesters is used to prepare cis-5-tert-butylproline. A concerted or nearly concerted metal carbenoid N-H insertion reaction mechanism is proposed.     

Preparation of 1,1,1,3,3-pentafluoropropane (HFC-245fa) by using a SbF5-attached catalyst

In this report, a simple process for preparing HFC-245fa through the reaction of 1,1,1,3,3-pentachloropropane (PCP) and anhydrous HF via two-step vapor-phase catalytic fluorination is described. The antimony pentafluoride catalyst was supported on inert porous materials to improve the catalytic activity. The resulting process catalyst not only exhibited high catalytic activity and excellent thermo-stability, but also improved the performance of SbF₅, in terms of hygroscopicity and corrosion.     

Separation of gallic acid from Cornus officinalis Sieb. et Zucc by high-speed counter-current chromatography

Gallic acid was separated from a n-butanol extract of the fruit of Cornus officinalis Sieb. et Zucc by high-speed countercurrent chromatography in two steps using two solvent systems composed of ethyl-acetate-ethanol n-butanol-water (5:1.8:6, v/v/v) and ethyl acetate-ethanol-water (5:0.5:6, v/v/v) successively. From 1 g of n-butanol extract the method produced 60 mg of gallic acid at a purity of 97%.     

The Study on the Thermal Stability of CLA in Egg Yolk

Conjugated linoleic acids (CLA) have been a subject of extensive investigation for their anticarcinogenic, hypolipidemic, antiatherosclerotic and immune-enhancing activities. Stability of CLA in foods has not received much attention by both academics and industry. Although CLA has shown many beneficial effects, its decomposition must be prevented when CLA in foods is processed, stored and transported. However, no study to date has addressed the stability of CLA in foods. The present study was carried out further to examine the stability of CLA in egg yolk during the storage and frying, using gas liquid chromatography (GLC) and silver ion high-performance liquid chromatography (Agt-HPLC). The eggs, containing 4.0% CLA per gramme of egg yolk, were 40s. Either storage for 6 months or frying for 40 s did not significantly change the composition of CLA in egg yolk. However, the degradation of CLA was statistically significant when the CLA components of egg yolk protected CLA from degradation. It is concluded that CLA is well preserved in egg before it is consumed.     

Chiral separation of N-(trans-4-isopropylcyclohexylcarbonyl)-D,L-phenylalanine isomers by high performance liquid chromatography

Summary A high-performance liquid chromatographic method was developed for the chiral separation of a new anti-diabetic agent, N-(trans-4-isopropylcyclohexylcarbonyl)-D-phenylalanine, and its L-enantiomer. The separation was performed on a Sumichiral OA-3300 column. Optimized mobile phase was 0.025 mol.L⁻¹ ammonium acetate in methanol solution. UV detection was at 210 nm. Baseline chiral separation was obtained within 12 minutes. The detection limits are 80 pg for the D-enantiomer and 120 pg for the L-enantiomer. RSD of the method was below 1% (n=5).     

Synthesis and analytical application of tribromocarboxyarsenazo as a new chromogenic reagent for zirconium

A new chromogenic reagent tribromocarboxyarsenazo has been synthesized and the chromogenic reaction of this reagent with zirconium studied. In the medium of 0.5 mol/1 HCl, a blue complex is formed by the reaction of zirconium with tribromocarboxyarsenazo. The maximum absorption of the complex is at 633 nm, and the apparent molar absorptivity is 4.8 x 10(4) 1/mol/cm. Beer's law is obeyed over the zirconium concentration range 0-18, mug/25 ml. The method has been applied to the determination of zirconium in aluminum, copper and magnesium alloys with satisfactory results.     

Anomalous Nitration Reactions of Halotropones and Tribromotropolone

Nitration of 2-bromo or 2-chlorotropone gave a new compound, 2,7-dinitrotropone: The halegen atom on the 2-position was displaced by the nitro group through an electrophilic substitution reaction. Nitration of 3,5,7-tribromotropolone gave 3,7-dibromo-5-nitropolone: the nitro group again displaced the bromine atom at position 5.     

Reduction and methyl transfer kinetics of the alpha subunit from acetyl coenzyme a synthase

Stopped-flow was used to evaluate the methylation and reduction kinetics of the isolated alpha subunit of acetyl-Coenzyme A synthase from Moorella thermoacetica. This catalytically active subunit contains a novel Ni-X-Fe4S4 cluster and a putative unidentified n = 2 redox site called D. The D-site must be reduced for a methyl group to transfer from a corrinoid-iron-sulfur protein, a key step in the catalytic synthesis of acetyl-CoA. The Fe4S4 component of this cluster is also redox active, raising the possibility that it is the D-site or a portion thereof. Results presented demonstrate that the D-site reduces far faster than the Fe4S4 component, effectively eliminating this possibility. Rather, this component may alter catalytically important properties of the Ni center. The D-site is reduced through a pathway that probably does not involve the Fe4S4 component of this active-site cluster.     

巯基葡聚糖凝胶分离富集光度法测定镉的研究

研究了在ＴｒｉｔｏｎＸ－１００存在下，新显色剂邻羧基苯基重氮氨基偶氮苯（ＣＤＡＡ）与镉的显色体系，在ｐＨ１０．６的Ｎａ２Ｂ４Ｏ７－ＮａＯＨ体系中，显色反应灵敏度很高。络合物的最大吸收位于５４５ｎｍ处，其摩尔吸光系数为２．２２×１０＾５Ｌ·ｍｏｌ＾－１·ｃｍ＾－１。镉含量在０￣１２μｇ／２５ｍＬ符合比耳定律。将该体系用于巯基葡聚糖凝胶分离富集－光度法测水样中微量镉，结果令人满意。