Crystal Structure of Trans-2-Amino-3-Cyano-4-(3',4'-Methylenedioxyphenyl)-1-Phenyl-2-Cyclopentene-r-1-ol

1INTRODUCTIONIntheearlyseventiesthreegroupsofinvestigators('--"establishedthatlow--va-lenttitanium,preparedbythereactionofstrongreducingagentsontitaniumtrichlo-rideortitaniumtetrachlorideintetrahydrofuran,canabstractoxygenfromketonesoraldehydes,leadingtotheformationofolefins.Anincreasinginterestinthereac-tioninducedbylow--valenttitaniumreagentsisobservedandalargenumberoffunc-tionalgroupscanbereducedt4--6).However,thereactionoflow-valenttitaniumreagentwith4,4--dicyano--1,3--diaryl--l-butano…     

Crystal Structure of 4, 5-trans-2-Amino-1, 3, 3-tricyano-4, 5-di (4-chlorophenyl)cyclopentene. Ethanol. Monohydrate

1mTRODUCT10NSincethetimeKaganhasdem0nstratedasimplepreparationofsamariumdiio-didefromsamariummetaland1,2-diiodoethanet1),SmI2hasbeenwidelyusedinsyntheticreactionst23.Thereactivityofsamariumdiiodidetowardsvariousnitrogen-containingcomP0undshasalreadybeenexamined.Thereare,toourknowledge,noliteratureexamplesforthereductionofcyanogrouptoproduceaminowiththisreagent.Inthispaper,wediscussedthecrystalstructureofthetitlecomP0undsyn-thesizedbythereactionofsamariumdii0didereagentwithp-chloroben-zyli…     

Synthesis and Molecular Structure of 5, 5-Dimethyl-2- (4' -methoxy)phenyl-1, 3, 2- thiazaphospholidine-4-thione 2-sulfide

1 INTRODUCTION In our previous study [1], we found that 1, 3, 2-thiazaphospholidine-4-thione 2-sulfide deriva- tives possessed various bioactivities such as herbicidal, antiviral, fungicidal activity, Which the is strongly held our interest to exploit new method for the synthesis of such phosphorohe- terocycles and investigate their biological activities. Different method for the preparation of 1, 3, 2-thiazaphospholidine-4-thione (one) 2-sulfides have been reported [2~4]. According to …     

X-ray Structure of 1- (3' -Phenyl-4' -morpholinyl-2' 5' - dithiole-1' - ylidene)-3, 4-biscarboethoxy-2-thionaphthalene

1INTR0DUCTIONa-Thiocarbonylthioformamideshavebeensynthesizedsince1980[l-23,however,thereisn0reP0rtofthesecomP0undsrelatedtheirpropertiesandreactivities(3).Ac-cordingtothepublishedpapers('-",adithioketone,adithioesterandadithioth-ioesteraresnitablefort4 2JcycloadditionwithalkenicandacetylenicdienophileS.Wewanttoknowwhethera-thiocarbonylthioformamideshavethesamecharacters,thereforethereactionofathiobenzoylthioformmorpholine(1)withdiethylacetylenedicarboxylate(2)wasexplored.Theredultsshowth…     

Synthesis and Structure of 6-(4- Fluorobenzylamino)-3-methylthio-1,5- diphenyl-1H-pyrazolo[3,4-d]pyrimidin-4(5H)-one

1 INTRODUCTION It was reported that the pyrazolopyrimidinone derivatives play a very important role in the bio- chemistry of living cell. Many potential drugs[1～3] and agrochemicals[4, 5] have been modeled on the compound, and the study on derivatives …     

Synthesis and Crystal Structure of N-[(3aR,4R,4aR,5aS,6S,6aS)-1,3-Dioxooctahydro-4,6-ethenocyclopropa[f]lisoindol-2(1H)-yl]-3-(trifluoromethyl)phenylmethanimine

The crystal structure of the title compound (C19H15F3N2O2, Mr= 360.33) was determined by single-crystal X-ray diffraction. The crystal belongs to triclinic, space group P(1), with a = 6.5604(7), b = 13.9614(16), c = 18.1790(18) (A), α = 102.749(7),β = 97.542(6), γ = 94.355(4)°, V= 1600.5(3) (A)3, Z = 4, Dc = 1.495 g/cm3, λ(MoKα) = 0.71070, F(000) = 744, μ(MoKα) = 0.122mm-1, R = 0.0434 and wR = 0.1051. A total of 7590 unique reflections were collected, of which 5429 with |F|2 ≥ 2σ|F|2 were observed. The two cyclohexene rings in the molecule adopt boat-boat conformations with the deviations of ring atoms C(9) and C10 from the C(5)/C(6)/C(7)/C(8) plane (Ⅰ) by 1.1204 (0.0023) and 1.1132 (0.0023) (A), respectively, whereas from the C(2)/C(3)/C(5)/C(8)plane (Ⅱ) by 1.1627 (0.0022) and 1.1818 (0.0021) (A), respectively. In the cyclopropane and lactam rings, atoms C(11) and N(1) point towards the double bond of C(9)-C(10) and the dihedral angle between the ring plane (Ⅲ) containing C(1), C(2), C(3) and C(4) and plane (Ⅳ) consisting of C(6),C(7) and C(11) is 55.76 (0.07)°. The dihedral angles between planes Ⅳ and Ⅰ and Ⅱ and Ⅲ are 63.58 (0.07)° and 58.10 (0.06)°, respectively. The dihedral angle between the benzene ring C(13)～C(18) and plane Ⅳ is 42.41 (0.06)°.     

Synthesis and Crystal Structure of Spiro[1-bromo(S)-4-(R)-hydroxy- 5-oxa-6-oxo-bicyclo[3.1.0]hexane-2,2''-(3''-diethyl-(-(S)-4''-Cl-benzyloxyphosphonyl-4''-(1R,2S,5R)-menthyloxybutyrolactone)]

The title compound, spiro[1-bromo(S)-4-(R)-hydroxy-5-oxa-6-oxo-bicyclo[3.1.0]-hxane-2,2'-(3'-diethyl-α-(S)-4'-Cl-benzyloxyphosphonyl-4'-(1R,2S,5R)-menthyloxybutyrolactone)] has been synthesized via the tandem asymmetric reaction and it crystallizes in a monoclinic system, space group P21 with a = 11.067(3), b = 12.484(2), c = 12.356(2)(A), β = 101.95°,C29H39BrC1O10P, Mr = 693.93, V= 1670.2(6) (A)3, Z= 2, Dc= 1.380 g/cm3, λ(MoKα) = 0.071073nm, μ = 1.410 mm-1, F(000) = 720, the final R = 0.0570 and wR = 0.0758 for 6190 observed reflections with I ＞ 2σ(I). The structure is characterized by the special combination of biologic phosphonyl group and one cyclopropane as well as two butyrolactones. The intermolecular hydrogen bond between O(3)-H(3A)…O(10) in the crystal lattice has been observed.     

Substituted N-picolylethylenediamines of the type (ArNHCH2CH2){(2-C5H4N)CH2}NR [R = Me, 4-CH2=CH(C6H4)CH2, (2-C5H4N)CH2] and their transition metal(II) halide complexes

Alkylation of (ArNHCH2CH2){(2-C5H4N)CH2}NH with RX [RX = MeI, 4-CH2=CH(C6H4)CH2Cl) and (2-C5H5N)CH2Cl] in the presence of base has allowed access to the sterically demanding multidentate nitrogen donor ligands, {(2,4,6-Me3C6H2)NHCH2CH2}{(2-C5H4N)CH2}NMe (L1), {(2,6-Me3C6H3)NHCH2CH2}{(2-C5H4N)CH2}NCH2(C6H4)-4-CH=CH2 (L2) and (ArNHCH2CH2){(2-C5H4N)CH2}2N (Ar = 2,4-Me2C6H3 L3a, 2,6-Me2C6H3 L3b) in moderate yield. L3 can also be prepared in higher yield by the reaction of (NH2CH2CH2){(2-C5H4N)CH2}2N with the corresponding aryl bromide in the presence of base and a palladium(0) catalyst. Treatment of L1 or L2 with MCl2 [MCl2 = CoCl2.6H2O or FeCl2(THF)1.5] in THF affords the high spin complexes [(L1)MCl2](M = Co 1a, Fe 1b) and [(L2)MCl2](M = Co 2a, Fe 2b) in good yield, respectively; the molecular structure of reveals a five-coordinate metal centre with bound in a facial fashion. The six-coordinate complexes, [(L3a)MCl2](M = Co 3a, Fe 3b, Mn 3c) are accessible on treatment of tripodal L3a with MCl2. In contrast, the reaction with the more sterically encumbered leads to the pseudo-five-coordinate species [(L3b)MCl2](M = Co 4a, Fe 4b) and, in the case of manganese, dimeric [(L3b)MnCl(mu-Cl)]2 (4c); in 4a and 4b the aryl-substituted amine arm forms a partial interaction with the metal centre while in 4c the arm is pendant. The single crystal X-ray structures of , 1a, 3b.MeCN, 3c.MeCN, 4b.MeCN and 4c are described as are the solution state properties of 3b and 4b.     

Synthesis and Crystal Structure of 2,3-Diethoxycarbonyl-4-phenyl-5-morpholinyl Thiophene

1INTRoDUCTIONa-Thiocarbonylthioformamidesweresynthesizedin198o[l~2i,however,thereisnoreportofthesecompoundsconcerningtheirpropertiesandreactionactivitiest33.Accordingtotheirstructure,theyseemtohavereactionwithdienophi1es,likesubsti-tutedolefinicandacetylenicdienophilestoleadcorrespondingDiels-Alderproduct.xylene(15ml),diethylbutynedioicester(O.2g,1.2mmol)wasadded,themix-turewasrefluxedfor20h,thencooledtoroomtemperatureandconcentrated.Theresiduewaspurifiedbysilicagelcolumnusingacetone/petr…     

Sulfur, tin and gold derivatives of 1-(2'-pyridyl)-ortho-carborane, 1-R-2-X-1,2-C2B10H10 (R = 2'-pyridyl, X = SH, SnMe3 or AuPPh3)

Reaction of the lithium salt of 1-(2'-pyridyl)-ortho-carborane, Li[1-R-1,2-C(2)B(10)H(10)](R = 2'-NC(5)H(4)), with sulfur, followed by hydrolysis, gave the mercapto-o-carborane, 1-R-2-SH-1,2-C(2)B(10)H(10) which forms chiral crystals containing helical chains of molecules linked by intermolecular S-H...N hydrogen bonds. The cage C(1)-C(2) and exo C(2)-S bond lengths (1.730(3) and 1.775(2)[Angstrom], respectively) are indicative of exo S=C pi bonding. The tin derivative 1-R-2-SnMe(3)-1,2-C(2)B(10)H(10), prepared from Li[1-R-1,2-C(2)B(10)H(10)] and Me(3)SnCl, crystallises with no significant intermolecular interactions. The pyridyl group lies in the C(1)-C(2)-Sn plane, oriented to minimise the NSn distance (2.861(3)[Angstrom]). The tin environment is distorted trigonal bipyramidal with axial N and Me. The gold derivative 1-R-2-AuPPh(3)-1,2-C(2)B(10)H(10), prepared from Li[1-R-1,2-C(2)B(10)H(10)] and AuCl(PPh(3)), reveals no NAu interaction in its crystal structure.     

Synthesis and Crystal Structure of 7,7- Dimethyl-2-amino-3-cyano-4-(3,4-methylenedioxylphenyl)- 5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran

1 INTRODUCTION Inorganic solid supports as catalysts resulting in higher selectivity, milder conditions and easier work-up has been reported as useful catalysts for many reactions [1~3]. Recently, we have reported the Knoevenagel condensation and some other reactions[4~6] catalyzed by KF-Al2O3. In this paper, we discussed the crystal structure of the title compound synthesized by the reaction of 2-cyano-3-(3,4-methylenedioxylphenyl)acrylonitrile and 5,5-dimethyl-1,3-cyclohexanedione in…     

Synthesis and Structural Characterization of [(η~5-C_5Me_5)_2Mo_2Fe_2S_4Br_2]

1 INTRODUCTION We once reported a CS bond cleavage reaction of (h5-C5Me5)Mo(StBu)3, which led to a Mo(IV) thio/thiolate complex (h5-C5Me5)MoS2(StBu)[1]. This reaction was facilitated by oxidants such as S8, gray selenium, and FeCl3[2]. The reaction with FeCl3 gave rise to a cubane cluster [(h5-C5Me5)2Mo2Fe2S4Cl2], which served as an excellent building block to construct various Mo/Fe/S clusters[2]. In this paper, we report the crystal structure of [(h5-C5Me5)2Mo2Fe…     

Synthesis and Structure of 4，5－bis（2，4－Dinitrophenylthio）－1，3－Dithiole－2－Thione

ＳｙｎｔｈｅｓｉｓａｎｄＳｔｒｕｃｔｕｒｅｏｆ４，５－ｂｉｓ（２，４－Ｄｉｎｉｔｒｏｐｈｅｎｙｌｔｈｉｏ）－１，３－Ｄｉｔｈｉｏｌｅ－２－ＴｈｉｏｎｅＱｕＺｈｅｎｇ；ＣａｉＪｉｎｇ－Ｈｕａ；ＦａｎｇＱｉ；ＹｏｕＸｉａｏ－Ｚｅｎｇ（Ｃｏｏｒｄｉｎａｔｉ...     

Synthesis and Crystal Structure of Tetramethyl 4aH-Pyrido [1, 2-a] Quinoline-1,2,3,4-Tetracarboxylate

1 INTRODUCTION Alkaloids and their derivatives are ubiquitous in natural products, and most of those compounds are of biological activities. Therefore, the structure modifi- cation of alkaloids is always the point that organic chemists and medicinal chemists focus on[1~10]. Qui- nolizine ring system is an important kind of alkaloid, which has a nitrogen atom shared by two six-mem- bered rings. Many medicines have quinolizine ring system, such as reserpine[11, 12] and berberine[13]. How- …     

Synthesis and Crystal Structure of 2[1-（1,1-Dimethylethyl）-5-methyl-1-H-pyrazol-4-ylcarbonyl]-N-phenyldrazinecarbothioamide

1INTRODUCTIONThiosemicarbazidespossessingNC=Sgroupareanessentialstructurefeatureresponsibleforvariousbiocidalproperties[1～7].Moreover,theyaretheconvenientandkeyintermediatesforthesyn-thesisofheterocycliccompoundssuchas1,3,4-thiadiazoles,1,2,4-triazoleand…     

Synthesis,Crystal Structure and Biological Activities of O-[（Z）-2-Methylbenzyl] 1-Phenyl-2-（1H-1,2,4-triazol-1-yl）ethanone Oxime

The crystal structure of the title compound （C18H18N4O, Mr = 306.36） has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with α = 4.783（0）, b = 13.577（1）, c = 13.830（1） A, α = 63.581（2）, β = 88.326（2）, γ = 86.161（2）°, V= 802.5（1） A3, Z= 2, Dc = 1.268 g/cm^3, F（000） = 324, μ（MoKa） = 0.082 mm^-1, the final R = 0.0497 and wR = 0.1199 for 3094 observed reflections （I 〉 2σ（I））. The dihedral angles between the phenyl （C（1）-C（4）-（6）） and triazole, the phenyl （C（13）-C（15）-C（18）） and triazole, and the two phenyl rings are 7.9（1）, 69.9（1） and 67.8（1）°, respectively. Strong C-H…π interaction joins molecules into a chain along the c axis and contributes to the stability of the structure. Preliminary bioassay results show that the title compound possesses excellent and selective fungicidal activity against Colletotrichum gossypii but displays moderate to weak insecticidal activity against aphides.     

Synthesis and Structure of Dinuclear Molybdenum Carbonyl Thiolate Compound[Et4N]2[Mo2(CO)8(SC6H4-CH3-p)2]

1　ＩＮＴＲＯＤＵＣＴＩＯＮＳｉｎｃｅｔｈｉｏｌａｔｅｌｉｇａｎｄｗａｓｉｎｔｒｏｄｕｃｅｄｉｎｔｏｍｏｌｙｂｄｅｎｕｍｃａｒｂｏｎｙｌｃｏｍｐｏｕｎｄｉｎ1 984 [1],ｔｈｅｉｎｖｅｓｔｉｇａｔｉｏｎｏｎｌｏｗ ｖａｌｅｎｃｅＭｏ -ＳＲｃｏｍｐｏｕｎｄｓｈａｓｒｅｃｅｉｖｅｄａｔｔｅｎｔｉｏｎｆｏｒｔｈｉｓｋｉｎｄｏｆｌｏｗ ｖａｌｅｎｃｅｃｏｍｐｏｕｎｄｓｐｏｓｓｅｓｓｃｅｒｔａｉｎａｄｖａｎｔａｇｅｏｎｃｏｍｐｏｕｎｄｓｙｎ ｔｈｅｓｉｓ,ｍｏｌｅｃｕｌｅｓｔｒｕｃｔｕｒｅａｎｄｐｈｙｓｉｃａｌａ…     

Dinitrogen functionalization with terminal alkynes, amines, and hydrazines promoted by [(eta5-C5Me4H)2Zr]2(mu2,eta2,eta2-N2): observation of side-on and end-on diazenido complexes in the reduction of N2 to hydrazine

Functionalization of the N2 ligand in the side-on bound dinitrogen complex, [(eta5-C5Me4H)2Zr]2(mu2,eta2,eta2-N2), has been accomplished by addition of terminal alkynes to furnish acetylide zirconocene diazenido complexes, [(eta5-C5Me4H)2Zr(C[triple bond]CR)]2(mu2,eta2,eta2-N2H2) (R = nBu, tBu, Ph). Characterization of [(eta5-C5Me4H)2Zr(C[triple bond]CCMe3)]2(mu2,eta2,eta2-N2H2) by X-ray diffraction revealed a side-on bound diazenido ligand in the solid state, while variable-temperature 1H and 15N NMR studies established rapid interconversion between eta1,eta1 and eta2,eta2 hapticity of the [N2H2]2- ligand in solution. Synthesis of alkyl, halide, and triflato zirconocene diazenido complexes, [(eta5-C5Me4H)2ZrX]2(mu2,eta1,eta1-N2H2) (X = Cl, I, OTf, CH2Ph, CH2SiMe3), afforded eta1,eta1 coordination of the [N2H2]2- fragment both in the solid state and in solution, demonstrating that sterically demanding, in some cases pi-donating, ligands can overcome the electronically preferred side-on bonding mode. Unlike [(eta5-C5Me4H)2ZrH]2(mu2,eta2,eta2-N2H2), the acetylide and alkyl zirconocene diazenido complexes are thermally robust, resisting alpha-migration and N2 cleavage up to temperatures of 115 degrees C. Dinitrogen functionalization with [(eta5-C5Me4H)2Zr]2(mu2,eta2,eta2-N2) was also accomplished by addition of proton donors. Weak Br?nsted acids such as water and ethanol yield hydrazine and (eta5-C5Me4H)2Zr(OH)2 and (eta5-C5Me4H)2Zr(OEt)2, respectively. Treatment of [(eta5-C5Me4H)2Zr]2(mu2,eta2,eta2-N2) with HNMe2 or H2NNMe2 furnished amido or hydrazido zirconocene diazenido complexes that ultimately produce hydrazine upon protonation with ethanol. These results contrast previous observations with [(eta5-C5Me5)2Zr(eta1-N2)]2(mu2,eta1,eta1-N2) where loss of free dinitrogen is observed upon treatment with weak acids. These studies highlight the importance of cyclopentadienyl substituents on transformations involving coordinated dinitrogen.     

Synthesis and Crystal Structure of [Copper(1,10-phenanthroline)_2(pyridine)]perchlorates

1 INTRODUCTIONThe molecular structures of five-coordinated copper (II) complexes show an extensive variability ranging from trigonal bipyramidal to square pyramidal stereochemistry, with most complexes displaying a structure which is intermediate between these two extremes[1,2]. Most crystal structures of 1,10-phenanthroline with copper (II) complexes are known, [Cu (phen)2X]Y, where X = Cl, Br, I, CN, NCS, H2O or thiourea and Y = perchlorate, nitrate, tetrafluoroborate, chloride o…     

Synthesis and Crystal Structure of 1-(o-methylphenyl)-2-(p-methoxyphenyl)-1,3,2-diazaphospholidin-4-thione-2-sulfide

11NTRODUCTIoNThederivativesofdiazaphospholidinoneorthecorrespondingthionesareknowntopossessinterestingbiologicalproperties,suchasherbicidalactivity"'2i.Inrecentyears,itwasreportedthatthel,4,2-diazaphospholindine-5-thione-2havegoodselectiveherbicidalactivity"'41.Tolookformoreeffectiveherbicideswithlowtoxicity,aseriesofnovel1-(o-methylphenyl)-2-(p-methoxyphenyl)-phospholidin-4-thione-sulfideshavebeensynthesizedandtheirmolecularstructuresstudied.PreliminarybioassaysshowthatthesecomPoundshaveg…