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.
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) , β = 102.253(3)o, C27H24FNO2, Mr = 413.47, Z = 4, V = 2119.9(8) 3, Dc = 1.296 g/cm3, 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.
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.
The crystal structure of the title compound (C26H33NO4 (C25.68H32.04N0.68O4.32, Mr = 419.35)) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space P21/c with a = 7.519(2), b = 28.933(5), c = 10.654(3) ?, β = 91.78(2)°, V = 2316.7(7) ?3, Z = 4, Dc = 1.202 g/cm3, μ = 0.081 mm-1, F(000) = 902, Mr = 423, the final R = 0.0424 and wR = 0.0911. In the structure, the pyridine ring adopts a boat conformation.
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.
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.
