Cp*Me5P6C5: Ein neues Carbaphosphan mit einem Strukturelement aus dem Hittorfschen Phosphor

Cp*Me₅P₆C₅: A New Carbaphosphane with a Structure Unit of Hittorf-Phosphorus The thermolysis of 1,2,3-tris(pentamethylcyclopentadienyl)cyclotriphosphane [(Cp*P)₃, 1 ] or 2,3,4,6-Tetrakis(pentamethylcyclopentadienyl)bicyclo[3.1.0]hexaphosphane [Cp*₄P₆, 2 ] leads in addition to the known 3,4-bis(pentamethylcyclopentadienyl)tricyclo[3.1.0.0^{2, 6}]hexaphosphane [Cp*₂P₆, 3 ] to the pentacyclic carbaphosphanes 3,4,5,6,11-pentamethyl-endo-9-pentamethylcyclopentadienyl- 3,4,5,6,11-pentacarba-pentacyclo [6.1.1^1,8.1^3,6.0^2,70^10,11]-4-en-undecaphosphane and 3,4,5,6,11-pentamethyl-exo-9-pentamethylcyclopentadienyl-3,4,5,6,11-pentacarba-pentacyclo [6.1.1^1,8.1^3,6.0^2,70^10,11]-4-en-undecaphosphane [Cp*Me₅P₆C₅, 4a, 4b ]. Furthermore, other polyphosphanes are formed, like 1,2,3,4-tetrakis(pentamethylcyclopentadienyl)cyclotetraphosphane [(Cp*P)₄, 5 ] and 2,4-bis(pentamethylcyclopentadienyl)-tetraphosphabicyclo[1.1.0]butane [(Cp*P)₂P₂, 6 ]. The structure of 4a and 4b is determined by NMR-spectroscopy. The molecule contains a P₅C₃-cunean-unit, to which a C₂Me₂-brigde and a PCp*-brigde is bonded.     

二羟基丙酮磷酸酯的合成

本文报道由3-氯-1,2-丙二醇(1)经七步反应,合成二羟基丙酮磷酸酯缩乙酮(7)的方法,总收率43%。在温和条件下,7可以水解为游离的二羟基丙酮磷酸酯(8)。     

Synthesis and Crystal Structure of N,N''''-Diphenyl-3, 6-diethyl-1,4-dihydro-s-tetrazine-1,4-dicarbonamide

1INTRODUCTIONIthasbeenarousedmoreandmoreinterestsinces-tetrazinewasfirstsynthesizedbyHautgschin1900[1].Thesynthesisofdihydroderivativeof3,6-dimethyl-s-tetrazinewasreportedindetailbySkorianetz[2].UsingX-ray,Jennison[3]foundthat1,6-dihydro-s-tetrazinehashom…     

对氟苯酚-过氧化氢-辣根过氧化物酶体系酶联荧光免疫分析研究──Ⅰ.对氟苯酚直接法及铝-钙指示剂偶合法测定人血清中乙肝表面抗原和表面抗体

对氟苯酚在辣根过氧化物酶（HRP）的催化下可被H2O2氧化，生成本酚及F-。测定对氟苯酚荧光猝灭程度及用铝－钙指示剂荧光体系检测酶促反应释放的F－，可分别建立HRP及其标记物的两种分析方法。铝－钙指示剂偶合法测定HRP的线性范围为0．031～31U／L，检测限（3δ）为0．0093U／L。两种方法分别用于测定人血清中乙肝表面抗原及抗体，结果令人满意。     

First synthesis of α-aminophosphonates from natural porphyrin derivatives by the Kabachnik—Fields reaction

A preparative procedure is proposed for the synthesis of α-aminophosphonates of natural porphyrins by the microwave-assisted Kabachnik—Fields reaction.__________Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 1, pp. 256–259, January, 2005.     

Stereoselective synthesis of procyanidin B3-3-O-gallate and 3,3″-di-O-gallate, and their abilities as antioxidant and DNA polymerase inhibitor

A simple method for the synthesis of procyanidin B3 substituted with a galloyl group at the 3 and 3″ position is described. Condensation of a benzylated catechin-3-O-gallate electrophile with a nucleophile, catechin and catechin-3-O-gallate, proceeded smoothly and stereoselectively to afford the corresponding dimer gallates, procyanidin B3-3-O-gallate and procyanidin B3-3,3″-di-O-gallate, in good yields. Further, their antioxidant activities on UV-induced lipid peroxide formation, DPPH radical scavenging activity and inhibitory activity of DNA polymerase were also investigated. Among three procyanidin B3 congeners (procyanidin B3, 3-O-gallate and 3,3″-di-O-gallate), the 3,3″-di-O-gallate derivative showed the strongest antioxidant and radical scavenging activity. Interestingly, the 3-O-gallate derivative was the strongest inhibitor of mammalian DNA polymerase with IC₅₀ value of 0.26 μM, although it showed the weakest antioxidant and radical scavenging activity. It became apparent that the presence of a galloyl group at the C-3 position in the proanthocyanidin oligomer was very important for biological activity, however, the antioxidant activity of these compounds was not parallel to the DNA polymerase inhibitory activity.     

微波溶样肉桂基荧光酮和表面活性剂连续荧光测定葡萄酒中铁和钴

观察到肉桂基荧光酮(略作CF)在pH≈8与Fc(Ⅲ)配位后荧光增强,CPB的加入使荧光更强,络合物与试剂荧光强度之比F_(FeR)/F_R随0～0.01μg/ml Fe(Ⅲ)线性变化,λ_(ex)=410nm,λ_(ex)=480nm;而CF在pH≈10与Co(Ⅲ)配位后荧光却减弱,乳化剂OP存在时使试剂荧光增强,若以荧光熄灭Co(Ⅲ)灵敏度便提高,试剂与络合物荧光强度之比F_R/F_(CoR)对0～0.016 μg/ml Co(Ⅲ)呈直线关系,λ_(ex)=300nm,L_(em)=352nm。控制化学条件和激发、发射波长,可不经分离测定葡萄酒(微波溶样)中铁和钴。     

5-Acyl-4-amino-2-phenyl-1,3-oxazin-6-ones

Intramolecular cyclization of acyl(ethoxycarbonyl)keteneN-benzoylaminals in boiling Ph₂O gives 5-acyl-4-amino-2-phenyl-1,3-oxazin-6-ones.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 7, pp. 1322–1323, July, 1995.This study was financially supported by the Russian Foundation for Basic Research (Grant No. 94-03-08964).     

RbEuI3和CsEuI3的合成及结构与性质研究

本文用一步法合成了新合物ＲｂＥｕＩ３与ＣｓＥｕＩ３，测定了化合物的组成，结构，熔点，密度，荧光光谱，极谱电位及磁矩，确定了化合物中Ｅｕ的价态为正二价。     

New stationary phases of conjugated π-electron systems for HPLC—characterization of structure and dynamics by solid state NMR spectroscopy

Four new stationary phases for HPLC were prepared by modifying silica gel with a trifrnctional aminoalkyl silane. A conjugated π-electron system was linked to the amino group either directly or with a carboxylic anhydride as a spacer in between. Characterization and dynamic measurements of the new stationary phases were performed by solid state NMR spectroscopy. The results of the ²⁹si and ¹³C CP/MAS techniques were compared with the recently developed ¹H MAS-only technique. Despite strong homonuclear dipole-dipole interactions it was possible to obtain well resolved ¹H MAS spectra of those stationaru phases with a high degree of crosslinking. Limited mobility of the aromatic ligand fragments is common for all examined stationaryu phases. The chromatographic properties of the new phases were tested by their ability tio sepatate a mixture of eight PAHS. It could be shown that the π-π interaction mechanism is responsible for the separation of the eight PAHs, because the elution order of the PAHs did not changem despite the use of both a nonpolar mobile phase (n-heptane) and a polar mobile phase (methanol/ water mixture).