The regioselective Mannich-type aminomethylation of hydroquinone afforded a nitrogen-containing compound, 2,5-bis-(morpholinomethyl)hydroquinone A, and its crystal structure was determined by single-crystal X-ray di...The regioselective Mannich-type aminomethylation of hydroquinone afforded a nitrogen-containing compound, 2,5-bis-(morpholinomethyl)hydroquinone A, and its crystal structure was determined by single-crystal X-ray diffraction. Crystal data for A: C16H24N2O4, Mr = 308.37, orthorhombic, space group Pbca, a = 10.479(4), b = 10.298(4), c = 14.865(5) ?, V = 1604.3(11) ?3, Z = 4, Dc = 1.277 g/cm3, F(000) = 664, μ = 0.092 mm-1, GOF = 1.078, the final R = 0.0508 and wR = 0.1075 for 1416 observed reflections with I > 2σ(I). There exist two intramolecular O–H…N hy- drogen bonds between the phenolic O atoms and the morpholine N donors and the morpholino rings assume the preferred chair conformation.展开更多
An aminophenol ligand, N,N,N＇-tri（2-hydroxy-5-methylbenzyl）-l,2-ethanediamine, was prepared through the Marmich reaction, and structurally characterized by NMR, IR, MS and single-crystal X-ray diffraction. The titl...An aminophenol ligand, N,N,N＇-tri（2-hydroxy-5-methylbenzyl）-l,2-ethanediamine, was prepared through the Marmich reaction, and structurally characterized by NMR, IR, MS and single-crystal X-ray diffraction. The title compound （C26H32N2O3, Mr = 420.54） belongs to the monoclinic system, space group P21/n with a = 8.6233（14）, b = 10.2655（16）, c = 26.017（4） A, β = 95.797（2）°, V = 2291.3（6） A^3, Z = 4, the final R = 0.0461 and wR = 0.1139 for 4267 unique reflections （Rint = 0.028） with 11691 observed ones （I〉 2a（I））.展开更多
6,8-Di-tert-butyl-3-（2,4-dimethyl-quinolin-7-yl）-3,4-dihydro-2H-benzo[e][1,3]oxa- zine（1） was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyd...6,8-Di-tert-butyl-3-（2,4-dimethyl-quinolin-7-yl）-3,4-dihydro-2H-benzo[e][1,3]oxa- zine（1） was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyde. The compound was structurally characterized by NMR, IR and single-crystal X-ray diffraction along with the elemental analysis. Compound 1 crystallizes as solvate with chloroform. The solvate 1·CHCl3（C28 H35 Cl3 N2 O, Mr = 521.93） belongs to the triclinic system, space group P1 with a = 10.852（2）, b = 11.352（2）, c = 13.050（3）, α = 101.95（3）, β = 92.94（3）, γ = 114.64（3）o, V = 1412.4（5）3, Z = 2, Dc = 1.227 g/cm3, F（000） = 552, μ = 0.347 mm–1, R = 0.0959 and wR = 0.2725（I 〉 2？（I））. The chloroform molecule displays a rotational disorder as one chloro atom can be located at two different positions. The packing of 1·CHCl3 was further stabilized by intramolecular C–H…O interactions, intermolecular C–H…N interactions, C–H…π interactions, and π…nteractions. The luminescent properties of compound 1 in both methylene chloride solution and the solid state were studied.展开更多
基金This work was financially supported by the Natural Science Foundation of Tianjin (No. 013606111)
文摘The regioselective Mannich-type aminomethylation of hydroquinone afforded a nitrogen-containing compound, 2,5-bis-(morpholinomethyl)hydroquinone A, and its crystal structure was determined by single-crystal X-ray diffraction. Crystal data for A: C16H24N2O4, Mr = 308.37, orthorhombic, space group Pbca, a = 10.479(4), b = 10.298(4), c = 14.865(5) ?, V = 1604.3(11) ?3, Z = 4, Dc = 1.277 g/cm3, F(000) = 664, μ = 0.092 mm-1, GOF = 1.078, the final R = 0.0508 and wR = 0.1075 for 1416 observed reflections with I > 2σ(I). There exist two intramolecular O–H…N hy- drogen bonds between the phenolic O atoms and the morpholine N donors and the morpholino rings assume the preferred chair conformation.
基金supported by Shandong Province Higher Educational Science and Technology Program (J09LB03)
文摘An aminophenol ligand, N,N,N＇-tri（2-hydroxy-5-methylbenzyl）-l,2-ethanediamine, was prepared through the Marmich reaction, and structurally characterized by NMR, IR, MS and single-crystal X-ray diffraction. The title compound （C26H32N2O3, Mr = 420.54） belongs to the monoclinic system, space group P21/n with a = 8.6233（14）, b = 10.2655（16）, c = 26.017（4） A, β = 95.797（2）°, V = 2291.3（6） A^3, Z = 4, the final R = 0.0461 and wR = 0.1139 for 4267 unique reflections （Rint = 0.028） with 11691 observed ones （I〉 2a（I））.
基金supported by the Frontiers of Science and Interdisciplinary Innovation Project of Jilin University(No.450060445023)Jilin Province Science and Technology Division(No.20100751)
文摘6,8-Di-tert-butyl-3-（2,4-dimethyl-quinolin-7-yl）-3,4-dihydro-2H-benzo[e][1,3]oxa- zine（1） was obtained by one-pot reaction starting from 2,4-di-tert-butylphenol, 7-amino-2,4- dimethyl-quinoline and paraformaldehyde. The compound was structurally characterized by NMR, IR and single-crystal X-ray diffraction along with the elemental analysis. Compound 1 crystallizes as solvate with chloroform. The solvate 1·CHCl3（C28 H35 Cl3 N2 O, Mr = 521.93） belongs to the triclinic system, space group P1 with a = 10.852（2）, b = 11.352（2）, c = 13.050（3）, α = 101.95（3）, β = 92.94（3）, γ = 114.64（3）o, V = 1412.4（5）3, Z = 2, Dc = 1.227 g/cm3, F（000） = 552, μ = 0.347 mm–1, R = 0.0959 and wR = 0.2725（I 〉 2？（I））. The chloroform molecule displays a rotational disorder as one chloro atom can be located at two different positions. The packing of 1·CHCl3 was further stabilized by intramolecular C–H…O interactions, intermolecular C–H…N interactions, C–H…π interactions, and π…nteractions. The luminescent properties of compound 1 in both methylene chloride solution and the solid state were studied.
