INFLUENCE OF TRACES OF WATER ON THE SYNTHESIS AND ELECTROLUMINESCENCE PROPERTIES OF POLY(2-METHOXY, 5- (2'''' -ETHYLHEXYL OXY)- 1, 4-PHENYLENE VINYLENE)

It was found that traces of water in the reaction medium would result in a great increase of gel and a decrease ofmolecular weight of the poly(2-methoxy, 5-(2'-ethylhexyloxy)-1, 4-phenylene vinylene) during the polymerization, whichultimately led to inferior film qualities and device properties. The device (ITO/PEDOT/MEH-PPV/Ba/Al) with MEH-PPVprepared under dry conditions has an external quantum efficiency of above 2.0%.     

RADICAL POLYMERIZATION OF N, N-DI(2-2''''-METHYL-ACRYLOYLOXY-PROPYL)-PARA-TOLUIDINE FUNCTIONAL MONOMER

Functional monomer (MP)_2PT having tertiary aromatic amino group was systhesized from the reaction of N, N-di (2-hydroxypropyl)-p-toluidine with 2-methyl acryloyl chloride. In the presence of organic peroxide, the radical polymerization of (MP)_2PT in toluene took place. The kinetics of (MP)_2PT polymerization and the ESR spectra of LPO-(MP)2PT-MNP systems were determined respectively.     

CRYSTAL AND MOLECULAR STRUCTURES OF TWO ISOMERS OF DIETHYL 2, 3-DICYANO-2, 3-DIPHENYLSUCCINATE

Diethyl 2, 3-dicyano-2, 3-diphenylsuccinate was prepared through the oxidative coupling of ethyl α-cyanophenylacetate with Cu~(++)-TMEDA-O_2 system. The product gave, upon chromatography, two crystalline compounds 1 and 2. The single crystals of 1 and 2 were identified by X-ray crystallographic analysis to be meso-and racemie-diethyl 2,3-dicyano-2,3-diphenylsuccinate respectively. It is noteworthy that in the molecules of 1 and 2 there is a remarkable lengthening effect of the bond length for the central C—C bond, i. e. 1: 1.585; 2: 1.62. It is also observed that there is steric hindrance between the substituent groups attached to the two carbon atoms of the central C—C bond respectively. These data provide the structural basis for the facile dissociation into radicals and the action of polymerization initiator of the title compound. CNDO/2 calculation of charge density and Wiberg bond order for compound 1 yields the results, which are consistent with the crystallographic data.     

DIELECTRIC PROPERTIES OF 1, 2-POLYBUTADIENES

The dielectric permittivity and loss tangent of 1,2-polybutadienes with different chain structures were determined as a function of temperature from-180℃ to 100℃ at different frequencies, and the frequency and structure dependence of the dielectric propertie of 1,2-polybutadienes have been investigated. It is found that a maximum of the permittivity occurs in the glass-transition region. The width of the glasstransition peak increases with increasing frequency while its height has little change. With a rise in the content of 1,2-units, the permittivity decreases and the height of the glass-transition peak slightly grows. A maximum of the width of the glass-transition peak appears when the content of 1,2-units is about 45%. Both the permittivity and dielectric loss drop down as the growth of the content of syndiotactic 1,2-units.     

SYNTHESIS, CHARACTERIZATION OF 2-[2-(3-NITRO-4-METHOXYLPHENYL) VINYLI-1-ME

ＳＹＮＴＨＥＳＩＳ，ＣＨＡＲＡＣＴＥＲＩＺＡＴＩＯＮＯＦ２－［２－（３－ＮＩＴＲＯ－４－ＭＥＴＨＯＸＹＬＰＨＥＮＹＬ）ＶＩＮＹＬＩ－１－ＭＥＴＨＹＬＰＹＲＩＤＩＮＩＵＭＰＥＮＴＡＡＮＤＨＥＸＡＮＩＴＲＡＴＯＲＡＲＥＥＡＲＴＨ（Ⅲ）ＣＯＭＰＬＥＸＥＳＨ...     

SYNTHESIS OF 2α,3α-DIHYDROXY-Δ4,7-6-KETOSTEROIDS, STRUCTURAL ANALOGS OF DIAULUSTEROLS A AND B

We studied various methods for synthesizing 2,3-dihydroxy- ^4,7 -6-ketosteroids, which are structural analogs of the ecdysteroids diaulusterols A and B.     

MECHANISM OF ELECTROCHEMILUMINESCENCE OF THE NEW REAGENT 6-(2-HYDROXY-DIETHYLAMINOPHENYLAZO)-2, 3-DIHYDRO-1, 4-PHTHALAZINE-1, 4-DIONE CATALYZED BY SILVER (Ⅰ)

The electrochemi luminescence of a new reagent 6-<2-hydroxy-4-diethylaminophenylazo>-2, 3-dihydro-1, 4-phthatazine-1, 4-dione in basic aqueous solution was studied. Trace amount of silver showed significant effect on the efficiency of light emission of HDEA during a positive trigonometrical wave pulse was exerted on the electrodes In the present paper, the ecl spectra of HDEA have been measured. λ_(max) is 410 nm. The reaction of HDEA chemiluminescence and the circular voltammetry, ultraviolet-visible spectrometry for the system have been investigated. The possible mechanism of the ecl of HDEA-KCL-KOH-Ag(I) system has been proposed.     

STUDIES ON DERIVATIVES OF 2, 3-DIHYDRO-4 H-1, 3, 2-BENZOXAZAPHOSPHORINE——THE DETERMINATION OF THE CRYSTAL AND MOLECULAR STRUCTURE OF 2, 3-DISUBSTITUTED-2, 3-DIHYDRO-4H-1, 3, 2-BENZOXAZAPHOSPHORIN-4-ONE (THION)-2-SULFIDE(OXIDE)

The two crystal structures of C_(17)H_(17),N_2O_2Cl_2PS (NP-8) and C_(17)H_(19)N_2O_2PS (NP-10-Ⅱ) have beendetermined by Patterson method. The crystals belong to monoclinic system with space group of P2_1/aand P2_1/n respectively. There are four molecules in the unit cell. Cell parameters: a = 26.622 (7)A, b = 7.711 (2) A., c = 9.461 (3) A, β = 94.90°(4) and a = 18.879(3) A, b = 10.199 (13) A, c = 8.948(3) A, β= 94.30°(3) for the two cells. After refinement by block diagonal matrix least squares me-thod, R factors are 0.046 for 2971 reflections of NP-8 and 0.076 for 1711 reflections of NP-10-Ⅱ. Referring to molecular structures of NP-8 and NP-10-Ⅱ spectra data have been satisfactorilycxplained. The characteristic features of the structures have been discussed.     

MOLECULAR STRUCTURE OF 2-[BIS(2-CHLOROETHYL)-AMINO]-6-BUTYLOXYMETHYL-TETRAHYDRO-2H-1, 3,2-OXA-ZAPHOSPHORINE-2-OXIDE

<正> The molecular structure of 2-[bis(2-chloroethyl)-amino]-6-t-butyloxymethyl-tetrahydro-2H-1,3,2-oxazaphosphorine-2-oxide has been determined by X-ray diffraction method.The crystal(C12H25Cl2NaO3P)is monoclinic with space group P21/a,a=11.965(2),b=10.335(3),c=14.543(5)A,β=102.24(2)°,V=1758(2)A3,Mr=347.22,Z=4,Dx=1.31 g/cm3,μ=4.66 cm-1,F(000)=736,R=0.051,Rw=0.054.The six-membered ring in this compound is in a distorted chair conformation with the t-butyloxymethyl group and the phosphoryl oxygen atom in equatorial positions which lead to cis-configuration.     

OXIDATION OF ALKYLBENZENES CATALYZED BY IRON( Ⅱ,Ⅲ)-1,10-PHENANTHROLINE AND 2, 2''''-BIPYRIDINE COMPLEXES

Oxidation of alkybenzenes PhCH_2R(R=H, CH_3, C_2H_5 and n-C_3H_7) under 1 atm. of O_2 or air catalyzed by iron(Ⅱ, Ⅲ)-2,2'-bipyridine and 1,10-phenanthroline complexes, affords the aryl-substituted ketones and alcohols with the conversion of 15.00％～34.58％ containing of 97.60％～99.80％ ketones and alcohols. The turnover numbers of these catalysts are over 3500 mol-cat. ~(-1)for 3.5 h.     

CRYSTAL STRUCTURE OF 2, 4-DITHIONE-3-AMINO-1, 3, 2-OX-AZAPHOSPHORINEBENZO-2-THIONO PYRIDINIUM

<正> The structure of title compound [C7H6N2OPS3]-·[HNC5H5]+ was determined by x-ray diffraction. It belongs to monoclinic system with space group P21/a, a = 16.745(2), b= 8.563(2), c=21. 050(5)(?), β=93.32(1)°, V= 3013. 6(?)3, Z = 8, Mr = 341. 4, F (000) = 1536, Dc=1. 504 g. cm-3,μ= 53. 0 cm-1. The crystal is composed of discrete cations C5H5NH+ and anions CrH6N2OPS3-. There are two pairs of the cations and the anions in each asymmetric unit. The stability of the anion is increased by the formation of (d-p)π bonding involving the 3d orbital of the P atom and the lone electron pairs of the S atoms.     

STUDY ON ASYMMETRIC SYNTHESIS OF 19-NORSTEROIDS SYNTHESIS OF A NEW OPTICALLY ACTIVE SYNTHON, (2R, 3S)-( )-2-ETHYL-2-(3'-OXO-4'-ENE)-AMYL-3-ACETOXY-CYCLOPENTANONE

This paper reports the synthesis of a new optically active synthon 6 for the asymmetricsynthesis of 19-norsteroids. Symmetric trione 9 obtained by the reaction of γ-carbonyl sulfo-xide 12b with 2-cthyl-1, 3-cyclopetanedione 8, was reduced asymmetrically by Saccharomycescerevisiae to (2R,3S)-(-)-14 and subsequently transformed into (2R,3S)-( )-6 by a shortreaction sequence. The absolute configuration of the asymmetrical product, (2R, 3S)-(-)-14,was established by converting it into the known compound (2R, 3S)-( )-17.     

SYNTHESIS OF 3-(2-QUINOLYL)TROPOLONES

3-Acetyltropolone was reacted with 2-aminobenzaldehydes to afford 3-(2-quinolyl)tropolones.2-Acetyl-7-methylaminotropone and 2-acetyl-7-ethylamino-tropone were respectively reacted with 2-aminobenzaldehydes to give the corres-ponding 2-(2-quinolyl)-7-methylaminotropones and 2-(2-quinolyl)-7-ethylaminotro-pones,which after treatment with sodium hydroxide solution also afforded 3-(2-quinolyl)tropolones.     

A HIGHLY EFFICIENT SYNTHESTS OF (2E)-α,β-UNSATURATED AMIDES

Ａ　ＨＩＧＨＬＹ　ＥＦＦＩＣＩＥＮＴ　ＳＹＮＴＨＥＳＴＳ　ＯＦ　（２Ｅ）－α，β－ＵＮＳＡＴＵＲＡＴＥＤ　ＡＭＩＤＥＳ￥ＪｉｎＸｉｎｇＤＵ；ＸｉａｎＨＵＡＮＧ（ＤｅｐａｒｔｍｅｏｔｏｆＣｈｅｍｉｓｔｒｙ，ＺｈｅｊｉａｎｇＮｏｒｍａｌＵｎｉｖｅｒｓｉｔ...     

CRYSTAL STRUCTURE OF 2-(BENZOYLMETHYLENE)HEXAHYDROPYHIMIDINE

<正> INTNDDUCTION. In our study on ketene aminals, it has been discovered that there are some differences between 2-(benzoylmethylene)imidazolidine and 2-(benzoylmethylene)hexahydropyrimidine in their reactivities and spectral data of NMR and IR. The crystal structure of the title compound was determined in order to carry out a systematic investigation on these problems.     

2-(2-ARYL-2-OXOETHYL)-4H-BENZO-1,4-THIAZIN-3-ONES AS PRODUCTS OF THE REACTION OF 2-AMINOTHIOPHENOL WITH β-AROYLACRYLIC ACIDS

Interaction of 2-aminothiophenol with β-aroylacrylic acids and their dibromo derivatives led to 2-(2-aryl-2-oxoethyl)-4H-benzo-1,4-thiazin-3-ones. The structure of synthesized compounds was confirmed by IR, ¹H, and ¹³C NMR spectra and X-ray analysis.     

DISPERSITY OF THE COPOLYMER OF STYRENE AND 2, 2, 6, 6-TETRAMETHYL-4-PIPERIDINYL-METHACRYLATE (PDS) IN POLYPROPYLENE AND ITS INFLUENCE ON PHOTOSTABILIZING ACTION OF PDS

The morphology of films of PDS/PP blends with various contents of PDS and with PDS of dif-ferent molecular weights was examined by scanning electron microscopy and the photostability ofthese films was studied by infrared spectrometry. Experimental results show that PDS is dispersedin PP matris as spherical globules being in size of the order of 10~(-1)μm when content of PDS is in therange of 0.1 % to 1%. The phase separation of PDS from PP results in decrease in photostabilizingaction of PDS to some extent. It is found that films of PP blended with PDS of different molecularweights show similar morphology and photostabilizing action if the content of PDS is kept constant.     

SYNTHESIS AND CHARACTERIZATION OF 2-(2-HYDROXY-3,5-DINITROPHENYLAZO)-7-(4-CHLORO-PHOSPHONPHENYLAZO)-1, 8-DIHYDROXY-NAPHTHALENE-3, 6-DISULF-ONIC ACID (CPAP) AS NEW REAGENT FOR DETERMINATION OF TOTAL PARE EARTHS

This paper reports the synthesis and general properties of the new reagent CPFP. Its dissociation constants have been determined. The characterization in determinating total RE with CPAP reagent has been investigated in detail. Analytic data for synthetic sample are satisfactory.     

5-芳酰氨基-2-苯基-2H-1, 2, 4-噻二唑-3-酮的合成

用1-芳酰基-5-苯基-2-硫代双脲与溴进行氧化成环反应制备了九个新的5-芳酰氨基-2-苯基-2H-1, 2, 4-噻二唑-3-酮, 相应的1-芳酰基-5-苯基-2-硫代双脲可以通过苯基脲与酰基异硫氰酸酯加成制得。     

SYNTHESIS OF PRECURSORS FOR NEW PYRIMIDINE ACYCLO-C-NUCLEOSIDE ANALOGUES BY RING TRANSFORMATION OF 2-FORMYLGALACTAL 1-2 *,†

Reactions of 2-formylgalactal 1, presented as an unsaturated sugar derivative with push-pull functionalization, with guanidinium and amidinium salts, respectively, were carried out under basic conditions to furnish the substituted 5-(1,2,4-tri-O-benzyl-d-lyxo-1,2,3,4-tetrahydroxybutyl)pyrimidines 2–4. Treatment of 1 with 2-aminobenzimidazole and 3-amino-1,2,4-triazole, respectively, afforded 3-(1,2,4-tri-O-benzyl-d-lyxo-1,2,3,4-tetrahydroxybutyl)benzo[4,5]imidazo[1,2-a]pyrimidine (5) and 6-(1,2,4-tri-O-benzyl-d-lyxo-1,2,3,4-tetrahydroxybutyl)-[1,2,4]triazolo[1,5-a]pyrimidine (6).