Synthesis and Crystal Structure of Methyl 3-（5- Bromo-1-ethyl-1H-indole-3-carbonyl）aminopropionate

Methyl 3-(5-bromo-1-ethyl-1H-indole-3-carbonyl)aminopropionate has been syn-thesized by the acylation of 5-bromo-3-trichloroacetylindole with β-alanine methyl ester,followed by alkylation with ethyl iodide,in 82.6% yield.Its crystal structure was gotten and determined by X-ray diffraction method.The crystal is of monoclinic,space group P2 1 /c with a=11.7927(8),b=14.9342(8),c=9.0060(5),β=101.558(6)°,V=1553.93(16)3,Z=4,D c=1.510 g/cm 3,λ=0.71073,μ(MoKα)=2.656 mm-1,M r=353.22 and F(000)=720.The structure was refined to R=0.0401 and wR=0.0825 for 1704 observed reflections with I > 2σ(I).In the crystal structure,intermolecular N(2)-H(2)···O(1) hydrogen bond and weak intermolecular bonds (C(1)-H(1) O(1) and C(10)-H(10B) O(2)) are formed,and π-π stacking also exists.     

Synthesis and Crystal Structure of （E）-ethyl 6-benzyl-2-[（cyclopropylmethylamino）（4-fluorophenylamino）-methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate

The crystal structure of the new title compound (E)-ethyl 6-benzyl-2-[(cyclopropylmethylamino)(4-fluorophenylamino)methyleneamino]-4,5,6,7-tetrahydrothieno[2,3-c]pyridine-3-carboxylate ethanol monosolvate (C28H31FN 4O2S·C2H6O, Mr=552.70) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic system, space group P21/c with a=13.806(10), b=10.850(7), c=19.938(14), β=98.842(9)° , V=2951(4)3 , Z=4, Dc=1.244g/cm 3 , F(000)=1176, μ=0.153 mm-1 , MoKα radiation (λ=0.71073), R=0.0758 and wR=0.2234 for 4262 observed reflections with I > 2σ(I). Intramolecular N-H…S and C-H…N interactions as well as intermolecular N-H…O and O-H…N hydrogen bonds help to stabilize the crystal structure. X-ray diffraction analysis reveals that the asymmetric unit contains one title molecule and one ethanol molecule.     

Synthesis, Crystal Structure, and Biological Activity of N-（ （ 1-cy clo h e xyl- 1H-tetrazo l-5-yl）（ 5-methyl- 1,2,3- thiadiazol-4-yl）methyl）-4-nitrobenzenamine

The title compound N-((1-cyclohexyl-1H-tetrazol-5-yl)(5-methyl-1,2,3-thiadiazol-4-yl) methyl)-4-nitrobenzenamine (C17H20N8O2S, Mr = 400.47) was synthesized via Ugi fourcomponents condensation reaction (U-4CR), and its structure was characterized by IR, 1H NMR, high-resolution mass spectrometry and single-crystal X-ray diffraction. The crystal belongs to orthorhombic, space group Pna21 with a = 20.390(2), b = 12.9660(14), c = 6.9399(8) , β = 90.00°, Z = 4, V = 1834.7(3)3, Mr = 400.47, Dc = 1.450 g/cm3, μ = 0.210 mm-1, F(000) = 840, R = 0.0348 and wR = 0.0717. X-ray analysis reveals that the dihedral angles formed between the thiadiazole and tetrazole rings, the benzene and tetrazole rings and the thiadiazole and benzene rings are 62.59, 86.73 and 70.07°, respectively. Three intermolecular hydrogen bonds N(1)-H(2)···N(6), C(4)-H(4B)···O(2) and C(17)-H(17)···N(3) are observed. Bioassay shows that the title compound has antifungal and antivirus activities against tobacco mosaic virus.     

Synthesis and Crystal Structure of （S）-Ethyl-2-（2-methoxy-phenylsulfenamido）-3-（1H-indol-3-yl）propanoate

With an aim to discover novel AHAS inhibitors,the title compound (S)-ethyl-2(2-methoxy-phenylsulfenamido)-3-(1H-indol-3-yl)propanoate (C 21 H 22 N 2 O 4 S,M r=398.47) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis.The crystal belongs to orthorhombic,space group P2 1 2 1 2 1 with a=8.078(2),b=12.824(4),c=18.788(6),V=1946.2(10) 3,Z=4,F(000)=840,D c=1.360 mg/m 3,μ=0.197 mm-1,the final R=0.0433 and wR=0.1035 for 3075 observed reflections with I > 2σ(Ⅰ).The absolute structure Flack parameter X of this compound is 0.00(8).A total of 14375 reflections were collected,of which 3431 were independent (R int=0.0437).X-ray analysis reveals that the crystal structure involves two intermolecular N-H···O and one N-H···S intermolecular hydrogen bonds with the neighboring molecules.The crystal structure was compared with our previously reported (S)-methyl 2-(4-R-phenylsulfonamido)-3-(1H-indol-3-yl)propanoate (R=H(1) and Cl(2)),which provided some useful information of these compounds.     

Synthesis,Crystal Structure and Biological Activity of 8-（（4-（（2,3-diaminopyridin-4-yl）oxy）-3-fluorophenyl）-amino）-2-（4-fluorophenyl）-3-methyl-2,7-naphthyridin-1（2H）-one

The new title compound 8-((4-((2,3-diaminopyridin-4-yl)-oxy)-3-fluorophenyl)-amino)-2-(4-fluorophenyl)-3-methyl-2,7-naphthyridin-1(2H)-one(C26H20F2N6O2, Mr = 486.48) has been prepared and determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 15.365(3), b = 13.144(2), c = 11.863(2), β= 108.882(3)°, Z = 4, V = 2267.0(7)3, Dc = 1.425 g/cm3, F(000) = 1008, μ = 0.105 mm-1, MoKa radiation(λ = 0.71073), R = 0.0480 and wR = 0.1294 for 3197 observed reflections with I 2σ(I). X-ray diffraction analysis reveals that the region C(substituents of 8-amino group and 3-methyl group on the 2,7-naphthyridin-1(2H)-one ring) of compound 6 are effectively planar. Intramolecular and intermolecular hydrogen bonds together with π···π interations are found in the structure. In addition, compound 6 shows potent c-Met and c-Kit kinase inhibition activities.     

Synthesis and Crystal Structure of N-[2-（4-Chlorophenyl）-1-（1-methylcarbamoyl-2-phenyl-ethylcarbamoyl）-3-phenyl-cyclopropyl]-benzamide

N-[2-(4-chlorophenyl)-1-(1-methylcarbamoyl-2-phenyl-ethylcarbamoyl)-3-phenyl-cyclopropyl]benzamide,C33H30ClN3O3,has been synthesized and characterized by IR,1H NMR,13C NMR and single-crystal X-ray diffraction.The crystal is of triclinic,space group P1 with a = 11.646(2),b = 13.795(3),c = 14.559(3),α = 76.422(4),β = 78.028(4),γ = 74.500(4)°,V = 2164.6(7)3,Z = 3,Mr = 552.05,Dc = 1.270 g/cm3,λ = 0.71073 ,μ(MoKα)= 0.171 mm–1,F(000)= 870,the final R = 0.0469 and wR = 0.0805 for 5554 observed reflections with I > 2σ(I).The N–H and oxygen atoms are involved in one-dimensional intermolecular hydrogen bonds,which further stabilize the structure.     

Synthesis,Crystal Structure and Antiproliferative Activity of 2-（（（5-（（（5,7-Dimethyl-[1,2,4]triazolo-[1,5-a]pyrimidin-2-yl）thio）methyl）-4-phenyl-4H-1,2,4-triazol-3-yl）thio）methyl）-4Hchromen-4-one Methanol Solvate

The novel crystal of the title compound 2-(((5-(((5,7-dimethyl-[1,2,4]triazolo-[1, 5-a]-pyrimidin-2-yl)thio)methyl)-4-phenyl-4H-1,2,4-triazol-3-yl)thio)methyl)-4H-chromen-4-one methanol solvate(C27H25N7O3S2, Mr = 559.66) has been prepared and its structure was determined by single-crystal X-ray diffraction. The crystal belongs to the monocline system, space group P21/c with a = 11.9879(9), b = 14.0743(10), c = 15.9706(11), β = 98.509(2)°, V = 2664.9(3)3, Z = 4, Dc = 1.395 g/cm3, F(000) = 1168, μ = 0.116 mm-1, MoKa radiation(λ = 0.71073), R = 0.0652, and wR = 0.1425 for 5220 observed reflections with I 2σ(I). X-ray diffraction analyses reveal that the molecule adopts a C-shape. The planes of the benzopyrone and triazolopyrimidine were nearly parallel to each other, with a dihedral angle of 1.21(3)°. Intramolecular and intermolecular hydrogen bonds together with π-π interations are found to exist in the structure. The results of MTT assay indicate that the title compound displays excellent antiproliferative activity against two human cancer cell lines.     

Synthesis and Crystal Structure of (E)-Ethyl (9-bromo-5-oxo-4-phenyl-1,10b-dihydro-5H-pyrano [3,4-c] chromen-2-ylidene) Acetate

The crystal structure of the title compound (C22H17BrO5 , Mr = 441.27) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic system, space group Pna21 with a = 11.76(1), b = 14.58(1), c = 11.52(1), V = 1973.93 , Z = 4, Dc = 1.485 g/cm3 , F(000) = 896, μ(MoKα) = 2.113 mm-1 , the final R = 0.0394 and wR = 0.0809 for 3918 observed reflections (Ⅰ > 2 (Ⅰ)). The single-crystal X-ray diffraction data indicate that the C=C bond is in an E-configuration. The intramolecular C(10)-H(10B)···O(4) and intermolecular C(17)-H(17)···O(4) hydrogen bonds contribute to the stability of the structure.     

Synthesis and Crystal Structure of 2,3,4,6-tetra-O-Acetyl-1-{4-chloro-3-[1-（4-ethoxyphenyl）-1-methylethyl]phenyl}-1-deoxy-β-D-glucopyranose

The title compound was synthesized and its crystal structure was determined by single-crystal X-ray diffraction.The crystal is of monoclinic system(C31H37ClO10,Mr = 605.06),space group P21 with a = 11.882(5),b = 10.106(5),c = 13.816(6),V = 1545.9(12)3,Z = 2,Dc = 1.300 g/cm3,F(000) = 640,μ = 0.179 mm-1,the final R = 0.0430 and wR = 0.0595 for 4960 observed reflections(I > 2σ(I)).The title compound was confirmed to be a β-anomer by single-crystal X-ray diffraction and 1H NMR.The proximal benzene ring is nearly orthogonal to the glucopyranoside ring,and the two benzene rings are also almost orthogonal to each other.Four non-classical intermolecular hydrogen bonds observed in the crystal lattice help to stabilize the crystal.     

Synthesis, Crystal, Calculated Structure and Biological Activity of N-（（6-bromo-2-methoxyquinolin-3-yl）（phenyl） methyl）-N-（1-adamantyl）-3-（dimethylamino） Propanamide

The halogenated hydrocarbon amination reaction between the original raw material N-((6-bromo-2-methoxyquinolin-3-yl)(phenyl)methyl)-3-chloro-N-(1-adamantyl) propanamide and dimethylamine hydrochloride produces the target molecule N-((6-bromo-2-methoxyquinolin-3- yl)(phenyl)methyl)-N-(1-adamantyl)-3-(dimethylamino) propanamide (C32H38BrN3O2, Mr = 576.56), and its structure was confirmed by elemental analysis, IR, 1H NMR, MS, and X-ray diffraction. This crystal is of monoclinic system, space group P21/c with a = 10.760(5), b = 14.768(5), c = 19.635(5), β = 113.969(16)°, V = 2851.0(18)3, Z = 4, Dc = 1.343 g/cm3, F(000) = 1208, μ(MoKα) = 1.475 mm-1, the final R = 0.0645 and wR = 0.2039. In total, 4681 independent reflections including 3164 observed ones with I > 2σ(I) were collected. The dihedral angle between substituted quinolyl and phenyl is 64.0°. Through C-H···O, C-H···N and C-H···Br weak hydrogen bonds among molecules, the whole molecule is stacked into a three-dimensional structure. The optimized geometric bond lengths and bond angles obtained by using density functional theory (DFT) have been compared with X-ray diffraction values. In addition, the preliminary biological test showed that the title compound has anti-Mycobacterium phlei 1180 activity.     

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 and Crystal Structure of （4S）-5-（2-Methoxy-2-oxoethylamino）-5-oxo-4-（3,4,5-trimethoxybenzamido） Pentanoic Acid

1 INTRODUCTION Aminopeptidase N (APN), a member of mem- brane-bound zinc-dependent exopeptidase, is known to be high expression on the brush border membran- es of the small intestine and renal proximal tubules[1]. The over-expression of APN has been involved in several pathological conditions including cancer[2], leukemia, diabetic nephropathy[3], rheumatoid arth- ritis[4], angiogenesis[5] and central nervous system di- seases, such as Alzheimer’s disease[6]. This has led to the sear…     

Synthesis and Crystal Structure of 3,3''-(2,2''-(Ethane-1,2-diylbis(oxy))bis(ethane-2,1-diyl))bis(2-(4-chlorophenylamino)quinazolin-4(3H)-one)

The title compound 3,3'-(2,2'-(ethane-1,2-diylbis(oxy))bis(ethane-2,1-diyl))bis(2- (4-chlorophenylamino)quinazolin-4(3H)-one) 3 (C34H30Cl2N6O4, Mr = 657.54) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in space group P1 with a = 9.9185(8), b = 10.6124(9), c = 15.4064(13) , α = 92.896(2), β = 103.813(2), γ = 94.635(2)°, V = 1565.5(2) 3, Z = 2, Dc = 1.395 g/cm3, μ = 0.257 mm–1, F(000) = 684, the final R = 0.0580 and wR = 0.1284 f...     

Synthesis, Crystal Structure and Fluorescent Properties of 1-（4-（Dimethylamino）benzylidene）- 4-（naphthalen- 1-yl） Thiosemicarbazide

1 INTRODUCTION Recently, for the fluorescent properties, Schiff base has been more and more important and widely studied in density optical memories, nonlinear op- tics (NLO), organic light-emitting diodes (OLED), polymer LED and electrogenerated chemilumines- cence (ECL)[1~5]. Thiosemicarbazones are a kind of Schiff bases with thiourea and good ligands easily chelating with transition metal ions. Although they have been studied extensively for a long time due to their chemical and b…     

Synthesis and Crystal Structure of Trans-4-[(5-(2,4-Dichlorophenoxy)-3-methyl-1-phenyl-1H-pyrazol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one

The title compound trans-4-[(5-(2,4-dichlorophenoxy)-3-methyl-1-phenyl-1H-pyra-zol-4-yl)methyleneamino]-1,5-dimethyl-2-phenyl-1,2-dihydropyrazol-3-one 3 (C28H23Cl2N5O2, Mr = 532.41) has been synthesized and its crystal structure was determined by single-crystal X-ray diffraction analysis. It crystallizes in triclinic, space group P1 with a = 8.9438(4), b = 11.6065(5), c = 14.2215(6) , α = 112.566(1), β = 92.324(2), γ = 102.91(1)o, V = 1315.65(10) 3, Z = 2, Dc = 1.344 g/cm3, μ(MoKα) = 0.282 mm-1, λ = 0.71073 , F(000) = 552, the final R = 0.0587 and wR = 0.1578 for 5071 observed reflections (I > 2σ(I)). X-ray analysis reveals that the product is a thermodynamically stable trans isomer. Intra-and intermolecular C(12)-H(12)···O(1) and C(28)-H(28)···O(1)#1 hydrogen bonds were observed in the title compound.     

Synthesis and Crystal Structure of N-(1,3,4-Thiadiazol-2-yl)-1-[1-(6-chloropyridin-3-yl)methy]-5-methyl-1H-[1,2,3]triazol-4-carboxamide

The crystal structure of the title compound (C12H10ClN7OS,Mr=335.78) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic,space group P1 with a=8.4093(11),b=9.4430(12),c=11.1454(14),α=95.508(2),β=111.366(2),γ=115.259(2)°,V=711.42(16) 3,Z=2,Dc=1.568 g/cm3,F(000)=344,μ(MoKα)=0.428 mm-1,the final R=0.0476 and wR=0.1243 for 2353 observed reflections (I > 2σ(I)). The dihedral angles between the pyridine and triazole,thiazole and triazole,and pyridine and thiazole rings are 69.2(1),9.2(1) and 72.7(1)o,respectively. Intramolecular C(8)-H(8B)…O(1) and N(5)-H(5A)…N(4) as well as intermolecular C(5)-H(5)…S(1),C(3)-H(3)…N(6) and N(5)-H(5A)…N(1) hydrogen bonds together with weak C-H…π hydrogen-bonding and π-π stacking interactions contribute to the stability of the structure. There is also evidence for significant electron delocalization in the triazolyl system.     

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 1-（4-Bromobenzoyl）-3- [5-（E）-styryl-1,3,4-thiadiazol-2-yl]urea

1 INTRODUCTION 1,3,4-Thiadiazole derivatives represent an interes- ting class of compounds possessing broad spectrum biological activities[1~4]. Aroyl ureas are known to exhibit diverse biological effects, such as insecticidal, fungicidal, herbicidal and plant growth regulating activities[5~8]. Therefore, it is worthwhile to investi- gate the compounds incorporating both 1,3,4-thiadia- zole nucleus and aroyl urea group. In the previous paper[9], a series of aroyl ureas containing 1,3,4-t…     

Synthesis and Crystal Structure of S-（＋）-N＇-Tertbutylaminocarbonyl-N- [3-methyl-2-（4-chlorophenyl）butyryl] Thiourea

The title compound S-( )-N'-tertbutylaminocarbonyl-N-[3-methyl-2-(4-chlorophenyl)butyryl] thiourea has been synthesized and its crystal structure was determined by singlecrystal X-ray diffraction an alysis. There exist intramolecular N(2)-H(2A)… O(1), C(17)-H(17A)…O(2) and N(3)-H(3A)…S(1) hydrogen bonds as well as intermolecular N-H…O interaction between the carbonyl and amidogen groups. Crystallographic data: C17H24ClN3O2S, Mr = 369.90,monoclinic, space group C2/c with a = 22.9922(19), b = 14.4844(12), c = 12.4618(11) (A),β =92.608(2)°, V= 4145.8(6) (A)3, Z = 8, Dc = 1.185 g/cm3, F(000) = 1568,μ(MoKa) = 0.298 mm-1, R =0.0578 and wR = 0.1308.     

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…