Synthesis,Crystal Structure,Fluorescence Properties and Geometrical Calculation of 4,8,10-Trimethyl-2-（3,5-dimethylpyrazol）-pyrido-[2＇,3＇：3,4]-pyrazol[1,5-a]-pyrimidin

A novel compound 4,8,10-trimethyl-2-(3,5-dimethylpyrazol)-pyrido-[2',3':3,4]-py-razol-[1,5-5-a]-pyrimidine(C17H18N6) has been synthesized from 2,6-dichloro-4-methylnico-tino-nitrile,hydrazine and acetylacetone by substitution and cyclolization.The structure was charac-terized by elemental analysis,1H NMR and IR,and single-crystal structure was determined by X-ray diffraction analysis.The compound crystallizes in the monoclinic system,space group P21/c with a = 8.0338(9),b = 28.618(3),c = 7.2688(8),β = 111.051(2)o,V = 1559.6(3) 3,Z = 4,Dc = 1.305 g/cm3,μ = 0.083 mm-1,Mr = 306.37,F(000) = 648,S = 0.971,the final R = 0.0795 and wR = 0.1746 for 1457 observed reflections(Ⅰ 2σ(Ⅰ)).The results demonstrate that the pyridine,pyrazole and pyrimidine rings are nearly coplanar,which is evident from the dihedral angles among the four rings in the range of 0.13～4.15o.The face-to-face π-π stacking interactions among pyridine,pyrazol and pyrimidine rings result in a supramolecular crystal,in which they seem to be effective in stabilizing the structure.Meanwhile,the fluorescence properties of the title compound were discussed,which showed very strong fluorescence.The calculated results(selected bond lengths,bond angles and torsion angles) are all typical and agree well with the experimental results,which demonstrates that B3LYP/6-31+G* is suitable for the title compound.     

Synthesis,Crystal Structure and Theoretical Calculation of [2-（2,6-Dioxacyclohexyl）-5-methoxylphenols]2

The title compound [2-（2,6-dioxacyclohexyl）-5-methoxylphenols]2 was synthesized by the reaction of 2-hydroxyl-3-methoxylbenzaldehyde and 1,3-propanediol in the presence of DMF-DMS adduct and characterized by IR spectrum, UV-Vis spectrum and X-ray crystallography. The title compound belongs to monoclinic, space group P21 with a = 9.8967（10）, b = 8.2240（9）, c = 13.3654（14） A^°, β= 90.016（2）°, C11H14O4, Mr = 210.22, V = 1087.8（2）A^°3, Z = 4, Dc = 1.284 Mg/m^3, F（000） = 448,μ = 0.098 mm^-1, the final R = 0.0300 and wR = 0.0761 for 2070 observed reflections with I 〉 2σ（I）. The molecules are connected via intermolecular O-H…O hydrogen bonds into a 2D network structure. Moreover, theoretical investigations of the title compound with HF/6-31G（d） method were performed, and its stability, frontier molecular orbital composition and Mulliken charge distribution were also discussed. The compound is a bis-molecule. The two molecules stay together and could not be separated. Two crystallographically independent molecules exist in an asymmetric unit. The bond lengths and bond angles of the two molecules are slightly different with each other.     

Synthesis and Crystal Structure of 2-(4''-Methylphenoxy)-5,8,9-trimethyl-3-phenyl Thieno[3'',2'':5,6]pyrido[4,3-d]pyrimidin-4-(3H)-one Hydrochloride

The title compound 2-(4′-methylphenoxy)-5,8,9-trimethyl-3-phenyl thieno[3′,2′:5,6]pyrido[4,3-d]pyrimidin-4(3H)-one hydrochloride (C26H23Cl4N3O2S, Mr = 583.33) has been deter- mined by single-crystal X-ray diffraction. The crystal belongs to monoclinic, space group P21/c with a = 14.8442(11), b = 11.5131(8), c = 17.2010(13) (A), β = 113.7250(10)o, V = 2691.3(3) (A)3, Z = 4, Dc = 1.440 g/cm3, S = 1.094, μ = 0.547 mm-1, F(000) = 1200, the final R = 0.0571 and wR = 0.1458. X-ray analysis reveals that the title compound combines with a molecule of dichloromethane by an intramolecular hydrogen bond. The thienopyridine ring is almost coplanar, and the dihedral angle between the thiophene plane and the pyridine plane is 0.6o.     

Synthesis and Properties of Derivatives of the new Heterocyclic System Benz[4,5]imidazo[1,2-c]pyrido[3',2';4,5]thieno[2,3-e]pyrimidine

Derivatives of a new heterocyclic system - benz[4,5]imidazo[1,2-c]pyrido[3',2';4,5]thieno[2,3-e]pyrimidine have been obtained by successive reactions in three stages - alkylation of 3-cyanopyridine-2(1H)-thiones with 2-chloromethylbenzylimidazole to give 2-benzimidazolylmethylthio-3-cyanopyridines, closing the thiophene ring in the latter to form 3-amino-2-(benzimidazolyl-2)thieno[2,3-b]pyridines, and cyclization of the pyrimidine ring by acylation with carboxylic acid anhydrides or chlorides.     

Synthesis and Crystal Structure of 8-(2,3-Dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo [f] cyclohepta [c] quinoline

The title compound 8-(2,3-dimethoxyphenyl)-10,11,12,13-tetrahydro-9H-benzo[f]-cyclohepta[c]quinoline(C26H25NO2,Mr=383.47) was synthesized and characterized by IR,1H NMR,13C NMR and elemental analysis.The crystal belongs to triclinic,space group P1 with a= 8.1490(16),b=9.2550(19),c=14.373(3) ,α=86.96(3),β=89.66(3),γ=70.32(3)°,Z=2,V=1019.2(4) 3,Dc=1.250 g·cm-3,μ(MoKα)=0.078 mm-1,F(000)=408,the final R=0.0555 and wR=0.1240 for 2228 observed reflections(Ⅰ > 2σ(Ⅰ)).X-ray analysis reveals that the seven-numbered ring is slightly similar to a six-numbered ring,forming the chair-like conformation.The four rings(Ⅰ,Ⅱ,Ⅲ and Ⅳ) in the benzo[f]cyclohepta[c]quinoline moiety form a screw structure.     

Condensed Thienopyrimidines. 14. Synthesis of 10H-Thiopyrano[4',3':4',5']thieno[2',3':4,5]pyrimido[2,3-c]-1,2,4-triazines

Reaction of a substituted 2-aminothienothiopyran with methyl(phenyl) isothiocyanate, intramolecular cyclization of the obtained N'-methyl(phenyl) thioureido derivatives, and work up of the cyclization products with hydrazine hydrate gave 2-hydrazinodihydrothiopyranothienopyrimidines. Treatment of the latter with pyruvic acid gave the novel 10H-thiopyrano[4',3':4',5']thieno[2',3':4,5]pyrimido[2,3-c]-1,2,4-triazines.     

Synthesis and Crystal Structure of 1-（4-Fluorophenyl）-2-hexylthiobenzo[4,5]-furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5（1H）-one

The crystal structure of the title compound 1-(4-fluorophenyl) -2-hexylthio-benzo [4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a]pyrimidin-5(1H) -one(C23H21FN4O2S,Mr = 436.5) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic,space group P21/n with a = 13.9854(3) ,b = 17.2678(4) ,c = 18.1828(5) ,β = 99.364(2) °,V = 4332.58(18) 3,Z = 4,Dc = 1.338,F(000) =1824,μ = 0.185 mm-1,MoKa radiation(λ = 0.71073) ,R = 0.0538 and wR = 0.1162 for 4728 observed reflections with I > 2σ(I) . X-ray diffraction analysis reveals the fused rings of benzo[4,5]furo[3,2-d]-1,2,4-triazolo[1,5-a] pyrimidin-5(1H) -one system are nearly coplanar. The crystal packing is mainly stabilized by weak intermolecular C-H···O hydrogen bond and π-π interactions.     

Synthesis and Crystal Structure of 2-Ethoxy-3-n-butyl-benzofuro[2,3-d]pyrimidin-4（3H）-one

The crystal structure of the new title compound 2-ethoxy-3-n-butyl- benzofuro[2,3d]pyrimidin-4（3H）-one （C16H18N2O3, Mr = 286.32） has been prepared and determined by singlecrystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 13.7167（14）, b = 13.113（1）, c = 8.378（1） A, β = 98.992（2）^o, V = 1488.4（3） A^3, Z = 4, Dc = 1.278, F（000） = 608, μ = 0.089 mm^-1, MoKa radiation （2 = 0.71073）, R = 0.0498, wR = 0.1238 for 2336 observed reflections with I 〉 2σ（I）. X-ray diffraction analysis reveals that all ring atoms in the benzo[4, 5]furo [2,3-d] pyrimi- dinone moieties are almost coplanar.     

Synthesis and THF Accompanied Crystal Structure of 11H-Naphtho[1',2':5,6]- pyrano[2,3-d]pyrimidin-11(10H)-one

8,9,12-Trihydro-9,9-pentamethylene-12-(3-nitrophenyl)-11H-naphtho[1',25,6]-pyrano[2,3-d]pyrimidin-11(10H)-one 1,another conversion product of Friedlndler reaction,has been synthesized by the reaction of 2-amino-4-(3-nitrophenyl)-4H-benzo[f]chromene-3-carbo-nitrile 2 with cyclohexanone in the presence of Lewis acid catalysts.The crystal of the title compound 1 THF solvate,C60H62N6O10,was obtained and determined by X-ray diffraction me-thod.The crystal is of triclinic,space group P with a = 11.4633(11),b = 12.6247(12),c = 19.658(2) ,α = 72.642(8),β = 89.045(9),γ = 68.340(5)°,V = 2509.6(4),Z = 2,Dc = 1.359 g/cm3,F(000) = 1088,Mr = 1027.16,the final R = 0.0674 and wR = 0.1869 with Ⅰ > 2σ(Ⅰ) and the goodness-of-fit S = 1.045 on F2.The pyrimidine ring has an envelope conformation,linked with a six-membered ring through a spiro C atom.The crystal packing of 1 THF solvate is stabilized by N-H···O hydrogen bonds,and π-π stacking interaction occurs between two adjacent nearly planar molecules of 1.     

Synthesis,Crystal Structure and Magnetic Behavior of a New Manganese（Ⅱ） Coordination Polymer [Mn（DPPZ）（PZDC）（H2O）] （DPPZ = Dipyrido[3,2-a：2＇,3＇-c] -phenazine and H2PZDC = Pyrazine-2,3-dicarboxylic Acid）

The title complex, [Mn（DPPZ）（PZDC）（H2O）] 1 （DPPZ = dipyrido[3,2 -a：2＇,3＇- c]phenazine and H2PZDC = pyrazine-2,3-dicarboxylic acid）, has been hydrothermally synthesized and structurally characterized by X-ray single-crystal diffraction, elemental analyses, IR, TG- DTA and magnetic susceptibility measurement. It crystallizes in triclinic, space group P1^- with a = 6.6842（5）, b = 7.5741（6）, c = 20.5755（15）A, α = 90.1160（10）, β = 97.0560（10）, γ = 97.3350（10）°, V= 1025.16（13）A^3, Z = 2, MnC24H14N6O5, Mr= 521.35, Dc= 1.689 g/cm^3, F（000） = 530, μ（MoKa） = 0.699 mm^-1, R = 0.0366 and wR = 0.0810. Compound 1 contains one- dimensional chains which are further stacked through π-π interactions to form a 3D supramolecular architecture. The water molecule O（1W） is involved in hydrogen bonding interactions with symmetric carboxylate oxygen atom 0（4） at （x＋ 1, y＋1, z） and symmetric PZDC nitrogen atom N（6） at （1-x, 1-y, 1-z）, which completes the structure of 1. Magnetic susceptibility measurement indicates that the compound behaves a weak antiferromagnetic exchange interaction.     

Crystal Structure of 1, 1-Dichloro-la, 3-diphenyl-1, la, 2, 3-tetrahydro-azirino [2, 1-d ] [1, 5]benzothiazepine (C_(22),H_(17)Cl_2NS )

1INTR0DUCTI0NBenzoheteroazepinecompoundsareimportantpharmaceuticalagents"-".Inre-centyears,ithasbeenfoundthatbenzoheter0azepinetricyclicderivatives,especiallythosefusedwithotherfiveorsix-memberedheterocycle,area1soofpotentialphar-maceuticalinterestst4-6j.Hence,muchattentionhasbeenpaidtothesynthesesofthem,suchasl,3-oxazino[3,2-djt1,5jbenzothia/diazepin-l-onet"'J,1,2,4-tria-zolo[4,3-dj[1,5jbenzothia/diazepine"',1,2,4-oxadiazolo[4,5-dj[l,5jbenzothia/diazepine',',andsoon.Meanwhiletheirstructur…     

Synthesis, Crystal Structure and Biological Activities of 3-[2-（4-Fluoro-phenyl）-ethyl]-5- methyl-4-hydroxyl-4-methyl-7-methylsulfanyl. 3,4-dihydro-pyrido[4,3-d]pyrimidine-8-carbonitrile

The title compound, 3-[2-(4-fluoro-phenyl)-ethyl]-5-methyl-4-hydroxyl-4-methyl- 7-methylsulfanyl-3,4-dihydro-pyrido[4,3-d]pyrimidine-8-carbonitrile, has been prepared and dete- mined by single-crystal X-ray diffraction. The crystal belongs to the triclinic system, space group P1 with a = 6.8754(8), b = 10.2617(12), c = 13.3491(16) , α = 93.163(2), β = 96.704(2), γ = 102.421(2)°, V = 910.35(19) 3, Z = 2, Mr = 370.44, Dc = 1.351 g/cm3, μ = 0.203 mm-1, F(000) = 388, the final R = 0.0573 and wR = 0.1497. X-ray analysis reveals that the pyridine and pyrimidine rings are almost coplanar.     

Synthesis and Crystal Structure of 2-Benzylamino-6-methyl-3-cyano-8- phenyl-5H-bispyrazolo[3,4-d,3'''',2''''-b]pyrimidine

1 INTRODUCTION The pyrazolopyrimidines have attracted conside- rable attention due to their versatile physiological activities, and a number of them exhibit excellent fungicidal[1], antiphlogistic[2～4] and antiumor[5] acti- vities. However, our interest in pyrazolo- pyrimidine stems is their applications as bactericide[6]. Herein we report the synthesis and structure of a tricyclic ring system bispyrazolo[3,4-d, 3?,2?-b]pyrimidine 1. 2 EXPERIMENTAL The 1H NMR spectra (CDCl3) were …     

Synthesis of Hexa- and Octahydropyrido[3'2':4,5]thieno[3,2-d]pyrimidines

The reaction of N-methylmorpholinium 4-(2-chlorophenyl)-5-cyano-2-oxo-1,2,3,4-tetrahydropyridine-6-thiolate with chloroacetamide in DMF in the presence of an excess of KOH gave 3-amino-2-carbamoyl-4-(2-chlorophenyl)-6-oxo-4,5,6,7-tetrahydrothieno[2,3-b]pyridine. Refluxing the latter with acyl chlorides in AcOH or heating in formic acid gave hexahydropyrido[3',2':4,5]thieno[3,2-d]pyrimidine derivatives and reaction with cyclohexanone gave a spiro-linked octahydropyrido[3',2':4,5]thieno[3,2-d]pyrimidine.     

4-[2-(4,6-二甲氧基-2-嘧啶氧基)苄胺基]苯甲酸正丙酯的合成和晶体结构

2-甲砜基-4,6二甲氧基嘧啶和N-(4-丙氧羰基苯基)-2-羟基苄胺在四氢呋喃溶液中反应, 生成标题化合物4-[2-(4,6-二甲氧基-2-嘧啶氧基)苄胺基]苯甲酸正丙酯,并测定了其晶体结构。该化合物分子式为C23H25N3O5,晶体属单斜晶系,空间群为P2/n,晶胞参数为a = 14.8504(8),b = 9.4420(4),c = 16.3129(9) 牛 = 104.881(1)埃琕 = 2210.6(2) 3,Z = 4,Dc = 1.272 g/cm3,F(000) = 896.00,(MoK? = 0.91 cm-1,R = 0.051,wR = 0.118,获得19761衍射数据,其中独立衍射点5004个。经元素分析、IR、MS和HNMR等对化合物的结构进行了表征。在分子结构中,各有3个不同的共轭平面。嘧啶环和苯环(C(7) C(12)),及苯环(C(14) C(19))的夹角分别为99.18 , 164.15埃?个苯环之间的夹角为94.93啊;衔锍世啻焦瓜蟆?     

四氢咪唑并[2',1':2,3]噻吩并[5,4-c]哌啶衍生物的合成及抗肿瘤活性

以4-哌啶酮为原料,经过胺基保护、缩合、环合、脱保护等步骤,设计合成了一系列新型的5,6,7,8-四氢咪唑并[2',1':2-3]噻吩并[5,4-c]哌啶类化合物。通过核磁共振波谱仪(~1H NMR、~(13)C NMR)、质谱(MS)和元素分析确证了其结构。对其体外活性研究发现,该类化合物对乳腺癌细胞MCF-7具有一定的抑制活性,其中化合物5a的抑制活性最为显著,半数抑制浓度(IC_(50))值达到了8.6μmol/L。为此类化合物的抗肿瘤活性研究提供了参考。     

Synthesis and Crystal Structure of 3-Benzyl-6-trichloromethyl-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazole

The title compound 3-benzyl-6-trichloromethyl-[1,2,4]triazolo[3,4-b][1,3,4]thiadiazole I （C11HTC13N4S, Mr = 333.62） has been synthesized, and its structure was determined by elemental analyses, IR, ^1H NMR, ^13C NMR, and X-ray diffractions. The crystal is of triclinic, space group P1^-, with a = 5.898（3）, b = 10.510（4）, c = 11.580（5） A, α = 74.936（7）, β= 75.476（7）, γ = 79.647（7）°, V= 665.9（5）/A^3, F（000） = 336, Z= 2, Dc = 1.664 g/cm^3, 2 = 0.71073A, p = 0.834 mm^-1, the final R = 0.0605 and wR = 0.0900. The secondary bonding interactions （SBIs） S…N and π-π stacking interactions are found in the crystal structure and they link the molecules into a three-dimensional network.     

Synthesis, Crystal Structure and Antidepressant Activity of 5-[4-(Benzyloxy)phenyl]-9-(n-propyl)-4,6-dioxa-1-azabicyclo[3.3.1]nonane Hydrochloride 0.5Hydrate

The title compound 2(C22H28N+O3)·H2O·2Cl-was synthesized by the reaction of 2-bromo-1-[4-(benzyloxy)phenyl]-1-pentone with 2,2'-azanediyldiethanol. The crystal determined by X-ray diffraction analysis belongs to the monoclinic system, space group Pc with a = 18.312(3), b = 14.838(3), c = 7.6227(14) , β = 97.981(4)°, Z = 2, Mr = 797.82, V = 2051.1(6) 3, Dc = 1.292 g/cm3, S = 0.956, μ = 0.21 mm-1, F(000) = 852, the final R = 0.0625 and wR = 0.1428 for 5683 observed reflections (Ⅰ > 2σ(Ⅰ)). Flack parameter is 0.10(9). The title compound is composed by four non-coplanar ring systems, two benzenes and two morpholines. One morpholine ring (C(3)-C(4)-N(1)-C(1)-C(2)-O(1)) forms a chair conformation, while the other (C(4)-C(3)-O(2)-C(6)-C(5)-N(1)) assumes a boat conformation. X-ray crystal structure displays extensive N-H…Cl and O-H…Cl intermolecular hydrogen bonds. The preliminary antidepressant activity test indicates that the inhibition ratio of SERT (5-HT Transporter) was 35.9% at the dosage of 10.0 mg/L.     

Synthesis and Crystal Structure of 1,3-Trans-1,4-cis- 3,4-di(4-bromophenyl)-1',2',3'-trihydro-1-hydroxy- benzo[g]bicyclo[3.3]octane-2-spiro-2'-indene-1'-one

1 INTRODUCTION Low-valent titanium reagents have exceedinglyhigh abilities to promote reductive coupling of car-bonyl compounds and they are attracting increasinginterest in organic synthesis[1]. Many other func-tional groups can also be coupled[2~8]. Recently, wehave reported some intermolecular reductive cou-pling reactions[9~12] and some new intramolecular re-ductive coupling reactions[13~16] induced by low-va-lent titanium reagents. The spiro[4.4]nonane skeleton has been found inmany…     

Synthesis and Crystal Structure of Ethyl （2-Amino-4-（2-chlorophenyl）-4H-benzo-[h]-chromene-2-yl） Formate

1 INTRODUCTION 2-Aminochromene is an important class of compounds as the main compounds of many natu- rally occurring products which can be used as cos- metics and pigments[1] and potential biodegradable agrochemicals[2～4]. Inorganic solid supports as c…