Synthesis and Crystal Structure of 1-Phenyl-3-methyl-4-（4-bromophenyl）-6-（2-chlorophenyl）pyrazolo[3,4-b] Pyridine under Microwave Irradiation

The title compound (C25H17BrClN3) has been synthesized by the reaction of 1-(2- chlorophenyl)-3-(4-bromophenyl)-2-propylene-1-one with 5-amino-3-methyl-1-phenyl pyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P1 with a = 9.3798(11), b = 10.6200(13), c = 11.7433(15) ?, α = 72.932(9), β = 78.877(10), γ = 72.045(9)o, V = 1057.0(2) ?3, Z = 2, Dc = 1.492 g/cm3, μ = 2.088 mm -1 , F(000) = 480, Mr = 474.78, the final R = 0.0428 and wR = 0.0879. X-ray analysis revealed that the dihedral angle between the pyrazol and pyridine planes is 6.45o.

Synthesis and Crystal Structure of 4-(2- Chlorophenyl)-5-cyano-3-methyl-6-oxo-1- phenyl-4,5,6,7-tetrahydropyrazolo[3,4-b] Pyridine under Microwave Irradiation

The title compound (C20H15ClN4O, Mr = 362.81) was synthesized by the reaction of ethyl 2-cyano-3-(2-chlorophenyl)-1-acylate with 5-amino-3-methyl-1-phenylpyrazole under microwave irradiation and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/n with a = 8.8192(19), b = 15.976(3), c = 13.094(3) ? = 103.074(4), V = 1797.1(7) ?, Z = 4, Dc = 1.341 g/cm3, = 0.229 mm-1, F(000) = 752, R = 0.0632 and wR = 0.1278. X-ray analysis reveals that the pyridine ring adopts an envelope conformation. The dihedral angle between the pyrazole and pyridine planes is 2.19, and inter- molecular hydrogen bonds are also observed in the molecule.

Synthesis and Crystal Structure of 1,7,7-Trimethyl-4-(4-methoxyphenyl)-4,6,7,8-tetrahydroquinoline-2,5(1H,3H)-diones under Microwave Irradiation

The title compound （C19H23NO3） was synthesized by the one-pot reaction ofp-methoxybenzaldehyde, Meldrum＇s acid, dimedone and CH3NH3Cl （NaOAc） in ethanol under microwave irradiation without catalyst and its crystal structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 8.7462（10）, b = 17.7367（19）, c = 11.5959（14） A, β = 110.981（3）°, V= 1679.6（3） A^3, Z = 4, Dc = 1.239 g/cm^3,μ（MoKa） = 0.083 mm^-1, F（000） = 672 and Mr = 313.38. The structure was refined to R = 0.0530 and wR = 0.1216. X-ray analysis reveals that the dihedral angle between plane 1 （N（1）, C（1）, C（2）, C（3）） and plane 2 （C（1）, C（2）, C（6）, C（7）, C（9）） is 3.64°, andt hat between plane 2 and plane 3 （C（11）～C（16）） is 85.33°.

Synthesis under Microwave Irradiation and Crystal Structure of 4-(3,4-Methylenedioxylphenyl)-6-methyl- 5-ethoxycaronyl-3,4-dihydropyrimidin-2(H)-one

The title compound 4-(3,4-methylenedioxylphenyl)-6-methyl-5-ethoxycaronyl-3,4- dihydropyrimidin-2(H)-one (C15H16N2O5) has been synthesized and determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P with a = 7.580(1), b = 7.920(2), c = 13.168(4) ? a = 96.44(2), b = 96.71(2), g = 109.81(2), V = 728.8(3) 3, Z = 2, Mr = 304.30, Dc = 1.387 g/cm3, F(000) = 320, m(MoKa) = 0.105 mm-1 (l = 0.71073 ?, R = 0.0446 and wR = 0.1205. In the molecule the pyrimidine ring adopts a boat conformation.

Synthesis and Crystal Structure of 9-（4-Methoxylphenyl）-1,8-di-oxo-3,4,5,6,7,9-hexahydroxanthene under Microwave Irradiation

The crystal structure of the title compound (C20H20O4, Mr = 324.36) has been determined by single-crystal X-ray diffraction. The crystal is of orthorhombic, space group Pbcn with a = 15.823(2), b = 18.002(3), c = 11.674(2) ?, V = 3325.34(67) ?3, Dc = 1.296 g/cm3, μ = 0.090 mm-1, Z = 8, F(000) = 1376, the final R = 0.0421 and wR = 0.0996. In the molecular structure, the pyran ring is of boat conformation, and the two six-membered rings fused with it adopt twisting-boat conformations.

Synthesis and Crystal Structure of N-methyl-9-(4-bromophenyl)-1,2,3,4,5,6,7,8,9,10-decahydroacridine-1,8-dione under Microwave Irradiation

The crystal structure N-methyl-9-(4-bromophenyl)-1,8-dioxo-1,2,3,4,5,6,7,8,9,10- decahydroacridine(C20H20BrNO2) was determined by single-crystal X-ray diffraction analysis. It belongs to P21/n space group, with a = 10.7999(18), b = 13.845(3), c = 11.4031(3) ?, β = 99.324(4)°, Dc = 1.525 g/cm3, Z = 4, λ = 0.71070 ?, μ(MoKα) = 2.455 mm-1, Mr = 386.28, V = 1682.5(5) ?3, F(000) = 792, the final R = 0.0463 and wR = 0.1053. In the crystal structure, the pyridine ring adopts a boat conformation, the two six-numbered rings fused with pyridine ring adopt twisting boat con- formation.

Synthesis and Crystal Structure of N-cyclopropyl-9 -(3,4-dicholophenyl)-1,2,3,4,5,6,7,8,9,10-decahydroacridine -1,8-dione under Microwave Irradiation

The N-cyclopropyl-9-（3,4-dicholophenyl）- 1,2,3,4,5,6,7,8,9,10-decahydroacri- dine-1,8-dione was synthesized by the reaction of 1,3-cyclohexanedione, N-cyclopropylamine and 3,4-dicholoaldehyde in water and glycol under microwave irradiation. Its crystal structure was determined by single-crystal X-ray diffraction analysis. It possesses P212121 space group, with a = 9.9103（5）, b = 13.3597（8）, c = 14.5633（8）A, V= 1928.16（18）A3 ,Mr = 402.30, Z = 4, Dc= 1.386 g/cm^3, 2 = 0.7107A,μ（MoKα）=0.354mm^-1 and F （000） = 840. The structure was refined to R = 0.0280 and wR = 0.0757. In the structure, the pyridine ring adopts a boat conformation.

Synthesis and Crystal Structure of Ethyl 4-(3,4-Methylenedioxylphenyl)-6-methyl-2-oxo-l,2,3,4-tetrahydropyridine-5-carboxylate under Microwave Irradiation

The crystal structure of the title compound (C16H17NO5) has been determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group C2/c with a = 18.520(2), b = 7.8910(1), c = 21.728(3) A, β = 104.77(1)°, V= 3070.4(7) A3, Mr= 303.31, Z = 8, Dc= 1.312 g/cm3, λ = 0.71073 A,μ(MoKα) = 0.098 mm-1 and F(000) = 1280. The structure was refined to R = 0.0486 and wR = 0.1287. There exist intermolecular hydrogen bonds in the crystal.

Microwave-assisted Syntheses and Crystal Structures of Benzimidazole Thiazolinone Derivatives

A rapid and efficient microwave-assisted synthesis method for the preparation of 3-（lH-benzo[d]imidazol-2-yl）-2-substituted phenyl thiazolidin-4-one （4a, 4b） was described. The structures of 4a and 4b were determined by elemental analyses, IR, 1H NMR and X-ray diffraction. In the crystals of compounds 4a and 4b, the imidazole ring and two benzene rings are planar. Interestingly, the dihedral angle between two benzene rings is 71.5° in 4a, while it is almost perpendicular in 4b due to the different benzene substituents. Meanwhile, the thiazolidinone ring is planar in 4a while slightly distorted with an r.m.s deviation of 0.1494（2） A in 4b. The hydrogen bonding interactions observed link the molecules to form a dimeric unit, which may be effective in the stabilization of the structure.

Microwave-assisted Synthesis and Crystal Structure of 3-Acetamido-1-phenyl-4-(2,6-dichloro)benzylidene-5-pyrazolone

The title compound,3-acetamido-1-phenyl-4-（2,6-dichloro）benzylidene-5-pyrazolone（C18H13Cl2N3O2,Mr = 374.21）,has been synthesized by one-step condensation of 2,6-dichloroben-zaldehyde with acetic anhydride and 3-amino-1-phenyl-5-pyrazolone under microwave irradiation.The compound was characterized by means of IR and 1H NMR.Its crystal and molecular structure were determined by X-ray diffractometry.It belongs to the orthorhombic system,space group Pbca,with a = 12.5312（13）,b = 8.5495（9）,c = 31.110（3） ,V = 3332.9（6） 3,Z = 8,Dc = 1.492 g/cm3,λ = 0.71073 ,μ（MoKα） = 0.407 mm-1,F（000） = 1536,the final R = 0.0394 and wR = 0.0984.A total of 15894 reflections were collected,of which 3630 were independent（Rint = 0.0362）.There exist three planes in the molecular structure.X-ray analysis reveals that the dihedral angles between planes 1 and 2,1 and 3 and 3 and 2 are 80.89,74.29 and 20.57°,respectively.

Synthesis and Crystal Structure of 2-Amino- 3-ethoxycarbonyl-4-(4-chlorophenyl)-4H, 5H-pyrano-[3,2-c]-benzopyran-5-one

The title compound 2-amino-3-ethoxycarbonyl-4-(4-chlorophenyl)-4H,5H-pyrano- [3,2-c]-benzopyran-5-one (C21H16ClNO5, Mr = 397.80) has been synthesized and characterized by X-ray crystallography. It crystallizes in triclinic, space group P1 with a = 5.756(1), b = 10.099(1), c = 17.106(3) ? a = 80.49(1), b = 83.13(1), g = 80.07(1), V = 961.8(2) ?, Dc = 1.374 g/cm3, = 0.231 mm-1, Z = 2, F(000) = 412, the final R = 0.0369 and wR = 0.0947. In the molecule the pyran ring is of boat conformation. The intermolecular hydrogen bonds of NH…O(5)(x+2, y+1, z+1) and NH…Cl (x+1, y1, z) as well as intramolecular hydrogen bond NH…O(5) are found.

Synthesis and Crystal Structure of 3,7,7-Trimethyl-1-phenyl-4-(3-nitrophenyl)-4,5,6,7,8,9-hexahydro-1H-pyrazolo[3,4-b]quinoline-5(6H)-one

The title compound (C25H24N4O3) has been prepared by the cyclocondensation of 5-amino-3-methyl-1-phenypyrazol, m-nitrobenaldehyde and dimedone in glycol under microwave irradiation without catalyst. The crystal structure was determined by single-crystal X-ray diffraction to be orthorhombic, space group Pbca with a = 16.3331(10), b = 13.8329(9), c = 19.4163(12) ?, V = 4386.8(5) ?3, Z = 8, Dc = 1.298 g/cm3, μ = 0.087 mm-1, F(000) = 1808, Mr = 428.48, the final R = 0.0519 and wR = 0.1019. X-ray analysis revealed that the pyridine ring is of boat conformation and the six-membered ring fused with it adopts twist boat conformation.② Corresponding author. Tu Shu-Jiang, born in 1957, professor, majoring in the synthesis of organic and heterocycle compounds. E-mail: laotu2001@ 263.net

Synthesis and Crystal Structure of 4-(4-Chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydropyrimidin-2(H)-one

The title compound 4-(4-chlorophenyl)-6-methyl-5-methoxy-caronyl-3,4-dihydro- pyrimidin-2(H)-one has been synthesized by the reaction of 4-chlorobenzaldehyde, methyl acetoa- cetate and urea using H3BO3 as a catalyst under microwave irradiation. Its structure was charac- terized by X-ray single-crystal diffraction techniques with the following data: triclinic, space group P1, a = 5.4513(4), b = 7.619(1), c = 16.118(4) ?, α = 80.42(1), β = 83.43(1), γ = 79.29(1)°, V = 646.19(19) ?3, Mr = 280.70, μ(MoKα) = 0.301 mm-1, Z = 2 and Dc = 1.443 g/cm3. In the molecule the pyrimidine ring is of boat conformation.

Synthesis and Crystal Structure of 3,3,6,6-Tetramethyl-N-hydroxy-9-ethyl-1,8-dioxo-1,2,3,4,5,6,7,8,9,10-decahydroacridine

The title compound (C19H29NO4) has been synthesized by the reaction of pro- paldehyde with dimedone and hydroxylamine hydrochloride in glycol under microwave irradiation, and its structure was determined by single-crystal X-ray diffraction. The crystal is of monoclinic, space group P21/c with a = 12.533(1), b = 13.184(2), c = 11.883(2) ?, β = 109.06(1)°, V = 1856.0(5) ?3, Mr = 335.43, Z = 4, Dc = 1.201 g/cm3, λ = 0.71073 ?, μ(MoKα) = 0.083 mm-1 and F(000) = 728. The structure was refined to R = 0.0488 and wR = 0.1456 for 2306 observed reflections with I > 2σ(I). X-ray analysis reveals that the pyridine ring adopts a boat conformation, while two cyclohexanone rings have envelope conformations.

Synthesis and Crystal Structure of 5-Cyclopropyl- 10-(4-fluorophenyl)-7,7-dimethyl-7,8-dihydro-5H- indeno[1,2-b]quinoline-9,11(6H,10H)-dione

The title compound 5-cyclopropyl-10-（4-fluorophenyl）-7,7-dimethyl-7,8-dihydro- 5H-indeno[1,2-b]quinolne-9,11（6H,10H）-dione was obtained by the reaction of 4-fluorobenzal- dehyde, 2H-indene-1,3-dione and 3-（cyclopropylamino）-5,5-dimethylcyclohex-2-enone in the presence of acetic acid under microwave irradiation. Its structure was confirmed by IR and 1H- NMR spectra. The crystal is of monoclinic, space group P21/c with a = 14.138（3）, b = 8.952（2）, c = 17.140（3）A, β = 102.253（3）°, C27H24FNO2, Mr = 413.47, Z = 4, V = 2119.9（8）A^3, Dc = 1.296 g/cm^3, μ（MoKα） = 0.087 mm^-1, F（000） = 872, the final R = 0.0425 and wR = 0.0905 for 2336 observed reflections （I 〉 2σ（I））. X-ray analysis revealed that the pyridine ring adopts a boat conformation and the six-membered ring fused with it assumes a twist boat conformation.

微波辐射下2-苄基苯并咪唑的合成和晶体结构

标题化合物C14H12N2在无溶剂条件下,用微波辐射法以盐酸作催化剂、邻苯二胺和苯乙酸为原料合成得到。最优化的合成条件是:n(邻苯二胺)∶n(苯乙酸)=1∶1.2(即邻苯二胺1.08 g,苯乙酸1.63 g),盐酸用量2mL,辐射时间8 min,微波功率480 W。用IR、1HNMR对产物进行了表征,并用单晶X射线衍射法测定了其单晶结构,标题化合物晶体属正交晶系,空间群Pbca,Mr=208.26,a=9.384 2(13)nm,b=9.723 4(13)nm,c=2.493 7(3)nm,V=2.275 4(5)nm3,Z=8,Dc=1.216 g/cm3,F(000)=880,μ=0.073 mm-1,GOF=1.001,R1=0.042 6,wR2=0.097 6〔Ⅰ>2σ(Ⅰ)〕。

4′-乙酰基苯并-15-冠-5缩氨基硫脲的微波合成及晶体结构

4′-acetylbenzo-15-crown-5thiosemicarbazone was synthesized with high yield (94%)via the reaction of 4′-acetylbenzo-15-crown-5 and thiosemicarbazide under the microwave irradiation and hydrochloric acid as the catalyst.Its structure was determined by single-crystal X-ray diffraction.The crystal belongs to triclinic crystal system,P-1 space group,a=9.5470(19)?,b=13.637(3)?,c=16.029(3)?,α=75.33(3)°,β=83.62(3)°,γ=70.99(3)°,V=1097.8(7)s assembled into supramolecule structure by intermolecular hydrogen bonds.

微波辐射下4-(2-氯苯基)-6-甲基-5-乙氧羰基-3,4-二氢嘧啶-2(H)-酮的合成和晶体结构

标题化合物C14H15ClN2O3是由2-氯苯甲醛、乙酰乙酸乙酯、尿素在TsOH作用下用微波辐射反应得到, 结构通过单晶X-射线衍射法确定, 其晶体属三斜晶系, 空间群P, Mr = 294.73, a = 7.688(1), b = 9.106 (2), c = 11.412(2) ? = 102.963(3), = 105.957(2), g = 102.484(2), V = 714.9(2) ?, Z = 2, Dc = 1.369 g/cm3, = 0.276 mm-1, F(000) = 308, 最终的偏离因子为R = 0.0845, wR = 0.2092。在分子结构中嘧啶环为船式结构, 平面1(苯环)与平面2 ((C(8)C(9) C(10)N(2))之间的两面角为 91.57啊?

1-苯基-3-甲基-4-(4-羟基-3-甲氧基)-苯甲叉-吡唑啉酮的微波合成和晶体结构

标题化合物C18H16N2O3是由香草醛和1-苯基-3-甲基-吡唑啉酮用微波辐射反应得到,结构通过单晶X-射线衍射法确定,其晶体属单斜晶系,空间群P21/c,Mr = 308.33, a = 21.101(4), b = 7.984, c = 20.076 ? = 115.81(1)? V = 3044.8(8) ? Z = 8, Dc = 1.345 g/cm3, = 0.093 cm-1, F(000) = 1296, 最终的偏离因子为R = 0.0403, wR = 0.0780, 分子之间存在氢键,形成了网状结构。

微波辐射下2,7,7-三甲基-3-乙氧羰基-4-(3-硝基苯基) -5-氧代-1,4,5,6,7,8-六氢喹啉的合成和晶体结构

标题化合物C21H24N2O5是由间硝基苯甲醛、达咪酮、乙酰乙酸乙酯、醋酸铵在微波辐射下干反应而得。结构通过单晶X-射线衍射法确定,其晶体属斜方晶系,空间群 Pbcn, a =17.953(3), b =15.206(4), c =14.299(3), V =3904.(2)3, Mr =384.42, Z =8, Dc =1.308g/cm3 , m(MoKa) =0.094mm-1, F(000)=1632。晶体结构用直接法解出,经全矩阵最小二乘法对原子参数进行修正,最终的偏离因子为R=0.0493, wR=0.1078。X-射线分析结果表明,吡啶环为船式构象,与之稠合的六元环为信封式构象。