The Preparation of 9-Methyl-3-thiophen-2-yl-thieno [3, 2-e] [1, 2, 4] triazolo [4, 3-c] pyrimi-dine-8-carboxylic acid ethyl ester is described. Elemental analysis, IR spectrum, 1H NMR, 13C NMR and X-ray crystal struct...The Preparation of 9-Methyl-3-thiophen-2-yl-thieno [3, 2-e] [1, 2, 4] triazolo [4, 3-c] pyrimi-dine-8-carboxylic acid ethyl ester is described. Elemental analysis, IR spectrum, 1H NMR, 13C NMR and X-ray crystal structure analyses were carried out to determine the composition and molecular structure of the title compound. There are two independent molecules in the asymmetric unit exhibiting intermolecular C-H…N, C-H…O interactions with additional π-π interaction that further helps in stabilizing the supramolecular structure. The results showed that the proposed method for synthesis is simple, precise and accurate which was further confirmed by crystal structure analysis.展开更多
The new uranyl complex UO2(NO3)2[PhN(CH3)C(O)(CH3)NPh]2 was synthesized and its crystal structure has been determined by single-crystal X-ray diffraction. Crystal data: C30H32N6O10U, triclinic, space group P with a = ...The new uranyl complex UO2(NO3)2[PhN(CH3)C(O)(CH3)NPh]2 was synthesized and its crystal structure has been determined by single-crystal X-ray diffraction. Crystal data: C30H32N6O10U, triclinic, space group P with a = 7.772(1), b = 9.267(1), c = 12.644(1) ? a = 68.246(8), b = 73.871(9), g = 84.99(1)o, V = 812.4(2) ?, Mr = 874.65, Z = 1, Dc = 1.788 g/cm3, F(000) = 426, m = 5.062 mm-1, the final R = 0.022 and wR = 0.059 for 3571 observed reflections (I > 2s(I)). The central uranyl ion is coordinated by six oxygen atoms, two from the carbonyl groups of N,N-dimethyl-N,N-dibenzenyl-urea molecules and the other four from two nitrate groups.展开更多
A stable organometallic Pd (Ⅱ) compound Pd(ptac-C,N)(acac-O,O) (Hacac = acetyl acetone, Hptac = 3-(2-pyridinethioxy)-acac, formula: C15H17NO4SPd, Mr = 413.76) 1 has been synthesized and its crystal structure was dete...A stable organometallic Pd (Ⅱ) compound Pd(ptac-C,N)(acac-O,O) (Hacac = acetyl acetone, Hptac = 3-(2-pyridinethioxy)-acac, formula: C15H17NO4SPd, Mr = 413.76) 1 has been synthesized and its crystal structure was determined by X-ray crystallography. The crystal is of monoclinic with space group C2/c, a = 17.9342(3), b = 17.7791(4), c = 13.1800(1) ? b = 128.400(1), V = 3293.5(1) 3, Z = 8, Dc = 1.669 g/cm3, F(000) = 1664, m = 1.269 mm-1, R = 0.0261 and wR = 0.0710 for 2653 observed reflections (I > 2s(I)). There exist two Pd rings in the title compound, C(14)O(4)PdO(3)C(12)C(13) and C(1)NPdC(8)S, with the palladium atom taking a square-planar coordination. Two oxygen atoms from the acetyl acetone ligand (PdO, 1.991(2) and 2.036(2) ), one N atom (PdN 2.019 ? and the g-carbon atom (PdC 2.067(3) ? from the ptac ligand are coordinated to Pd.展开更多
文摘The Preparation of 9-Methyl-3-thiophen-2-yl-thieno [3, 2-e] [1, 2, 4] triazolo [4, 3-c] pyrimi-dine-8-carboxylic acid ethyl ester is described. Elemental analysis, IR spectrum, 1H NMR, 13C NMR and X-ray crystal structure analyses were carried out to determine the composition and molecular structure of the title compound. There are two independent molecules in the asymmetric unit exhibiting intermolecular C-H…N, C-H…O interactions with additional π-π interaction that further helps in stabilizing the supramolecular structure. The results showed that the proposed method for synthesis is simple, precise and accurate which was further confirmed by crystal structure analysis.
基金This work was supported by the Funds of the Key Laboratory of Organic Syntheses of Jiangsu province (No. KJS01018) and the Funds of Young Teachers of Suzhou University
文摘The new uranyl complex UO2(NO3)2[PhN(CH3)C(O)(CH3)NPh]2 was synthesized and its crystal structure has been determined by single-crystal X-ray diffraction. Crystal data: C30H32N6O10U, triclinic, space group P with a = 7.772(1), b = 9.267(1), c = 12.644(1) ? a = 68.246(8), b = 73.871(9), g = 84.99(1)o, V = 812.4(2) ?, Mr = 874.65, Z = 1, Dc = 1.788 g/cm3, F(000) = 426, m = 5.062 mm-1, the final R = 0.022 and wR = 0.059 for 3571 observed reflections (I > 2s(I)). The central uranyl ion is coordinated by six oxygen atoms, two from the carbonyl groups of N,N-dimethyl-N,N-dibenzenyl-urea molecules and the other four from two nitrate groups.
基金the State Key Basic Research and Development Plan of China (001CB108906), the NNSF of China (No. 29733090 and No. 20173063), Key Project in KIP of CAS (KJCX2-H3) and the NSF of Fujian province (E0020001)
文摘A stable organometallic Pd (Ⅱ) compound Pd(ptac-C,N)(acac-O,O) (Hacac = acetyl acetone, Hptac = 3-(2-pyridinethioxy)-acac, formula: C15H17NO4SPd, Mr = 413.76) 1 has been synthesized and its crystal structure was determined by X-ray crystallography. The crystal is of monoclinic with space group C2/c, a = 17.9342(3), b = 17.7791(4), c = 13.1800(1) ? b = 128.400(1), V = 3293.5(1) 3, Z = 8, Dc = 1.669 g/cm3, F(000) = 1664, m = 1.269 mm-1, R = 0.0261 and wR = 0.0710 for 2653 observed reflections (I > 2s(I)). There exist two Pd rings in the title compound, C(14)O(4)PdO(3)C(12)C(13) and C(1)NPdC(8)S, with the palladium atom taking a square-planar coordination. Two oxygen atoms from the acetyl acetone ligand (PdO, 1.991(2) and 2.036(2) ), one N atom (PdN 2.019 ? and the g-carbon atom (PdC 2.067(3) ? from the ptac ligand are coordinated to Pd.
文摘将经过多级破碎分选所得的废线路板粉末过60目筛,以2 mol/L HCl溶液、超纯水洗涤,并用丙酮脱水。将预处理后的滤渣、滤纸填入萃取池,或者用新滤纸包裹后置于索氏提取管内,添加5μL内标物,分别用加速溶剂萃取法(ASE)或索氏提取(SE)法进行萃取,依次采用多层硅胶柱和活性炭柱对萃取提取物进行净化、洗脱,得到二噁英测试样品。用同位素稀释-高分辨气相色谱-质谱联用仪分析样品中二噁英的含量。考察两种提取方法及不同氯代数对15种^(13)C-2,3,7,8-PCDD/Fs回收率的影响,比较两种方法的准确度和精密度。结果表明,ASE和SE对15种^(13)C-2,3,7,8-PCDD/Fs的回收率分别为54.3%~113.0%和28.3%~77.7%,实测废线路板中二噁英毒性当量(Toxic equivalent quangtity,TEQ)分别为0.075 ng TEQ/kg和0.266 ng TEQ/kg。在方法精密度允许范围内,ASE相对具有简单快速、溶剂用量少和准确的优势。
