The title compound Ph3P=C（H）C（O）PhNO2 （L） has been prepared by the addition of triphenylphosphine in acetone as solvent to 2-bromo-1-（3,nitrophenyl）ethanone followed by the addition of alkaline solution of sod...The title compound Ph3P=C（H）C（O）PhNO2 （L） has been prepared by the addition of triphenylphosphine in acetone as solvent to 2-bromo-1-（3,nitrophenyl）ethanone followed by the addition of alkaline solution of sodium hydroxide. The yellow crystals of the title ylide were grown in methanol/chloroform solution by drop method without stirring at room temperature. The solid state structure of ylide has been established by X-ray crystallography analysis. In the molecule of the title compound, the geometry around the P atom is nearly tetrahedral and the O atom is in synperiplanar orientation to the P atom. The nitrophenyl ring is twisted with respect to the plane of the carbonyl group through an angle of 36.6（1）°. The crystal （C26H20NO3P, Mr = 425.40） belongs to the monoclinic system, space group P21/n with a = 10.889（3）, b = 14.467（3）, e = 13.872（4）A, β = 103.08（3）°, V = 2128.6（10） A3, Z= 4, T= 100（2） K, R = 0.059 and wR = 0.163 for 3984 observed reflections with I〉 2σ（I）.展开更多
A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux cond...A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux conditions. 3,12-dimethylbenzo[a]quinoxalino[2,3-c] phenazine with bidentate character reacts with mercury（II） bromide to give suitable crystals. All products were confirmed by IR, ^1H and ^13C NMR, and the metal complex by single-crystal X-ray method. The crystal（C24H16Br2HgN4, Mr = 720.82） belongs to the triclinic system, space group P1 with a = 10.186（6）, b = 10.421（6）, c = 11.470（7） A, α = 98.670（7）, β = 95.069（7）, γ = 109.831（7）°, V = 1119.4（12） A3, Z = 2, Dc = 2.139 Mg/m^3, μ = 10.46 mm^-1, F（000） = 676, R = 0.043 and wR = 0.115 for 3982 observed reflections with I 〉 2σ（I）.展开更多
文摘The title compound Ph3P=C（H）C（O）PhNO2 （L） has been prepared by the addition of triphenylphosphine in acetone as solvent to 2-bromo-1-（3,nitrophenyl）ethanone followed by the addition of alkaline solution of sodium hydroxide. The yellow crystals of the title ylide were grown in methanol/chloroform solution by drop method without stirring at room temperature. The solid state structure of ylide has been established by X-ray crystallography analysis. In the molecule of the title compound, the geometry around the P atom is nearly tetrahedral and the O atom is in synperiplanar orientation to the P atom. The nitrophenyl ring is twisted with respect to the plane of the carbonyl group through an angle of 36.6（1）°. The crystal （C26H20NO3P, Mr = 425.40） belongs to the monoclinic system, space group P21/n with a = 10.889（3）, b = 14.467（3）, e = 13.872（4）A, β = 103.08（3）°, V = 2128.6（10） A3, Z= 4, T= 100（2） K, R = 0.059 and wR = 0.163 for 3984 observed reflections with I〉 2σ（I）.
文摘A new series of quinoxalinophenazine derivatives were synthesized in good yields by the reaction of 2,3-dibromonaphthalene-1,4-dione with different aryl-1,2-diamines in DMF as solvent at 120-130℃ or under reflux conditions. 3,12-dimethylbenzo[a]quinoxalino[2,3-c] phenazine with bidentate character reacts with mercury（II） bromide to give suitable crystals. All products were confirmed by IR, ^1H and ^13C NMR, and the metal complex by single-crystal X-ray method. The crystal（C24H16Br2HgN4, Mr = 720.82） belongs to the triclinic system, space group P1 with a = 10.186（6）, b = 10.421（6）, c = 11.470（7） A, α = 98.670（7）, β = 95.069（7）, γ = 109.831（7）°, V = 1119.4（12） A3, Z = 2, Dc = 2.139 Mg/m^3, μ = 10.46 mm^-1, F（000） = 676, R = 0.043 and wR = 0.115 for 3982 observed reflections with I 〉 2σ（I）.
