Synthesis and Crystal Structure of exo-4-（3,4-Dichlorophenyl）-8-ethyl-3,3a,4,5,8, 12d-hexahydro-2H-furo[3,2-c]indolo[3,2-f]quinoline

The title compound exo-4-(3,4-dichlorophenyl)-8-ethyl-3,3a,4,5,8,12d-hexahydro-2H-furo[3,2-c]indolo[3,2-f]quinoline (C25H22Cl2N2O, Mr = 437.35) was synthesized and crystallized. The crystal belongs to tetragonal, space group I4(1)/a with a = 17.4903(3), b = 17.4903(3), c = 28.3403(5) , Z = 16, V = 8669.6(3) 3, Dc = 1.340 g·cm-3, μ(MoKɑ) = 0.319 mm-1, F(000) = 3648, R = 0.0429 and wR = 0.711 for 2714 observed reflections I > 2σ(I). X-ray analysis reveals that atoms C(1), C(2), C(3), C(4), C(5) and N(1) on the new pyridine ring are slightly distorted, forming a distorted boat conformation.     

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 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…     

Syntheses and Crystal Structures of 4-Amino-3- （3-hyd roxyp ropyl）- 1H-1,2,4-triazole-5（4H）-thione and 6-（4-Biphenylyl）-3-（3-hydroxypropyl）-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazine

1INTRODUCTION It has been reported that3,6-disubstituted-7H-1,2,4-triazolo[3,4-b][1,3,4]thiadiazines have a broad spec-trum of bioactivities,such as antimicrobial[1],antibac-terial,antifungal[2],anti-inflammatory[3],diuretic[4],an-thelmintic and analgesic[5].They can also be used as plant-growth regulating agents[6],photographic coup-lers,dyes for improved preservability and absorption characteristics,and inhibitors of malignant cellularZOU K.H.et al.:Syntheses and Crystal Structures o…     

Synthesis and Crystal Structure of Ethyl（2-amino-4-（3-nitrophenyl）-1,4-dihydro-2H-pyrano[3,2-h]quinolin-3-）carboxylate

1 INTRODUCTION 2-Aminochromene is an important class of com- pounds found as the main compounds of many naturally occurring products employed as cos- metics and pigments[1] and utilized as potential biodegradable agrochemicals[2～4]. The utility of fluoride salts as potential base in variety of syn- thetic reactions has been recognized in recent years[5, 6]. However, low solubility of fluoride salts in ordinary solvents limits their wide applications in organic syntheses. On the other ha…     

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 Crystal Structure of Methyl(7,7-Dimethyl-2-amino-4-(4-chlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran-3-yl)Carboxylate

<正>The title compound methyl (7,7-dimemyl-2-amino-4-(4-chlorophenyl)-5-oxo-5,6,7,8-tetrahydro-4H-benzo-[b]-pyran-3-yl) carboxylate (C19H20ClNO4, Mr = 361.81) was synthesized and crystallized. The crystal belongs to triclinic, space group P 1 with a = 8.519(2), b = 10.346(2), c = 11.481(3) A, α = 108.16(1), β = 107.78(2), γ= 91.83(2)°, Z = 2, V = 906.5(3) A3, Dc = 1.326 g/cm3, μ(MoKα) = 0.234 mm-1, F(000) = 380, R = 0.0467 and wR = 0.1270 for 3142 observed reflections (I > 2σ(I)). X-ray analysis reveals that the C(7), C(8), C(9), O(1), C(10) and C(11) atoms form a six-membered ring which adopts a boat conformation. In the ring, the distances of C(8)-C(9) and C(10)-C(11) are 1.332(3) and 1.357(3) A, respectively, which indicates that they are C=C double bonds. Another six-membered ring (C(8)-C(9)-C(15)-C(14)-C(13)-C(12)) adopts the half-chair confonnation. In addition, there are intermolecular hydrogen bonds in the crystal structure.     

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, 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, Structure and Biological Activities of 2-Methylthio-3-cyano-7-（4-methoxyphenyl）- pyrazolo[1,5-a]pyrimidine

1INTRODUCTION Pyrazolo[1,5-a]pyrimidine derivatives have shown various biological activities in the terms of antibac-terial,antischistosomal and xanthine oxidase inhibi-tors[1~5].The enaminones are highly reactive inter-mediates and have been extensively used as build-ing blocks in organic synthesis especially in the he-terocyclic compounds[6~8].In addition,a great deal of interest has been focused on the synthesis of py-razolo[1,5-a]pyrimidine through versatile enamino-nes because of thei…     

Synthesis,Crystal Structure and Anti-tumor Activity of 2-（2-Chloro-4-nitrophenyl）-4- （4-chlorophenyl）-3a,4-diethoxy-2,3,3a, 4-tetrahydrochromeno[3,4-d] [ 1,2,3]diazaphosphole

The title compound 2-（2-chloro-4-nitrophenyl）-4-（4-chlorophenyl）-3a,4- diethoxy- 2,3,3a, 4-tetrahydrochromeno[3,4-d][1,2,3]diazaphosphole 2 （C29H30Cl2N3O7P, Mr = 633.44） was synthesized and its structure was characterized by IR, MS, ^1H NMR, ^13C NMR, ^31p NMR, elemental analysis and single-crystal X-ray diffraction. It crystallizes in triclinic, space group P1^-, a = 9.1549（3）, b = 10.7168（4）, c = 17.6272（6）A, α = 102.9363（12）, β = 90.2713（9）, γ = 117.4265（10）°, V= 1484.41（9）A^3, Z= 2,μ（MoKa） = 0.323, F（000） = 658, Z= 2, De= 1.417 g/cm^3, the final R = 0.0687 and wR = 0.2066 for 4943 observed reflections （I 〉 2σ（I））. X-ray analysis reveals that the diazaphospholine ring is almost planar and the two ethoxy groups bonded on the 3a- and 4-positions are in trans configurations. Its antiproliferative activity was also tested in vitro against four human tumor cell lines.     

2-氨基-3-氰基-4-(4-氟苯基)-4H-苯并[h]苯并吡喃的合成和晶体结构

标题化合物与N,N-二甲基甲酰胺(DMF)形成的1:1混合结晶物C20H23FN2OC3H7NO由对氟苯甲醛、丙二腈、-萘酚在六氢吡啶存在下合成并经DMF与水的混合溶剂重结晶而得, 其结构通过元素分析、IR 和1H NMR对化合物进行了表征,用X-射线单晶衍射法测定了该化合物的晶体结构。结果表明,晶体属于单斜晶系,P21/n空间群,a = 6.365(1), b = 10.620(2), c = 29.122(6) ? b = 92.00(1), V = 1967.3(6) ?, Mr = 389.42, Z = 4, Dc = 1.315 g/cm3, m (MoKa) = 0.092 mm-1, F(000) = 816。晶体结构用直接法解出,经全矩阵最小二乘法修正,最终偏离因子R = 0.047, wR = 0.1053。化合物分子中,原子C(1), C(2), C(3), C(4), C(5) 和O(1)形成1个六员环,该六员环中C(1)C(2)键长为1.346(3) 牛砻魑肆被肺焦瓜蟆?     

Synthesis and Crystal Structure of Ethyl 2-Methylthio-7-phenylpyrazolo[1,5-a]pyrimidine-3-carboxylate

The crystal structure of ethyl 2-methylthio-7-phenylpyrazolo[l,5-a]pyrimidine-3- carboxylate (C16H15N3O2S, Mr = 313.37) has been determined by single-crystal X-ray diffraction analysis. The crystal belongs to monoclinic, space group P21/n with a = 19.361(7), b = 7.595(3), c = 20.910(8) (A), β = 94.925(6)°, V= 3064(2) (A)3, Z = 8, Dc= 1.359 g/cm3,μ = 0.222 mm-1, F(000) = 1312, R = 0.0546 and wR = 0.1082 for 5374 unique reflections with 3419 observed ones (I ＞ 2σ(I)). The results show that all ring atoms in the pyrazolopyrimidine moiety are coplanar with strong tensile force. The structure analysis indicates that the single crystal contains strong nonclassical hydrogen bonds.     

Synthesis and Crystal Structure of 3-（4-Chlorophenyl）-8-cyano-2-（di-isopropylamino）-5-methyl-7-（methylthio）-pyrido[4,3-d]pyrimidine-4（3H）-one

The crystal structure of the new title compound 3-(4-chlorophenyl)-8-cyano-2-(di-iso-propylamino)-5-methyl-7-(methylthio)-pyrido[4,3-d]pyrimidine-4(3H)-one(C22H24ClN5OS,Mr = 441.97)has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic,space group Pna21 with a = 7.6721(5),b = 18.9370(11),c = 15.6260(9),V = 2270.2(2)3,Z = 4,Dc = 1.293 g/cm3,F(000)= 928,μ = 0.283 mm-1,MoKa radiation(λ = 0.71073 ),R = 0.0494 and wR = 0.1062 for 3278 observed reflections with I > 2σ(I). X-ray diffraction analysis reveals that all ring atoms in the py-ridopyrimidinone moiety are almost coplanar. Intramolecular C(20)-H(20)···N(4),C(19)-H(19A)···N(3),C(18)-H(18C)···N(3)and C(16)-H(16B)···O(5)hydrogen bonds together with weak C···π interactions are found in the structure.     

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 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 and Crystal Structure of 2-（ 4-Decarboxydehydroabietyl）- 5-p-tolyl-[ 1,3,4 ]-oxadiazole

2-（4-Decarboxydehydroabietyl）-5-p-toyl-[1,3,4]-oxadiazole, C28H34N2O, has been synthesized and characterized by IR, NMR, elemental analysis and single-crystal X-ray diffraction method. The crystal belongs to the orthorhombic system, space group P212121 with a = 6.1351（5）, b = 14.8495（19）, c = 25.9050（2） A, V = 2360.0（4） A3, Z = 4, Mr = 414.57, Dc = 1.167 Mg/m^3, 2 = 0.71073 A,μ（MoKa） = 0.070 mm^-1, F（000） = 896, the final R = 0.0452 and wR = 0.1076 for 1647 observed reflections with I 〉 2σ（I）. There are five rings in the crystal structure of the title compound, but the oxadiazole ring is non-coplanar with the benzene ring D.     

5-取代氨基-12-取代苯并[c]菲啶衍生物的合成、晶体结构及生物活性

为了寻找新的高活性农药, 利用2-甲基苯甲腈与不同的醛反应, 再通过2,3-二氯-5,6-二氰基-1,4-苯醌(DDQ)脱氢或NaH和CH3I氮甲基化, 合成了3个系列共18个5-取代氨基-12-取代苯并[c]菲啶衍生物, 其中15个是未见文献报道的化合物. 它们的结构均经1H NMR, 13C NMR, IR和高分辨质谱表征; 用X射线衍射测定了化合物5-氨基-12-(4-二乙氨基苯基)-11,12-2H-苯并[c]菲啶盐酸盐(3c)的晶体结构. 初步的生物活性测试结果表明, 部分化合物具有一定的杀菌活性和促进黄瓜子叶生根活性.     

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 Crystal Structure of 2,10-Di-tert-butylindolo[3,2,1-jk]carbazole

The title compound, 2,10-di-tert-butylindolo[3,2,1-jk]carbazole (C26H27N, Mr=353.49), has been synthesized by palladium-catalyzed intramolecular arylation and characterized by 1H NMR, 13C NMR and X-ray crystal structure determination. The crystal crystallizes in the monoclinic system, space group P21/c with a=13.6409(5), b=11.6706(4), c=13.1678(5), β=100.6180(10)°, V=2060.39(13)3 , Z=4, Dc=1.140 mg/m3 , μ=0.065mm-1 , F(000)=760, the final R=0.0456 and wR=0.1209 for 3012 observed reflections (I > 2σ(I)).