Amino acid benzyl ester p-toluenesulfonic acids were synthesized under microwave irradiation condition by reaction of four amino acids with benzyl alcohol and p-toluenesulfonic acid,and then reacted with the N-phthalo...Amino acid benzyl ester p-toluenesulfonic acids were synthesized under microwave irradiation condition by reaction of four amino acids with benzyl alcohol and p-toluenesulfonic acid,and then reacted with the N-phthaloyl-L-glutamic anhydride to yield compound 3a-d,hydrogenised and treated with NH3(g) to obtain the target compounds—thalidomide ammonium salt derivatives.The microwave-assisted method was used to synthesis the thalidomide amino acid benzyl ester p-tolunensulfonic acid,the reaction time was brought down with improved yield as compared with conventional heating method.The structures were comfirmed by MS,1H-NMR and elemental analysis.展开更多
The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amin...The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amine with 2-methoxylcarbonylbenzene-sulfonylisocya- nate. The crystal is of monoclinic, space group P21/c with a =11.169(3), b = 9.508(3), c = 17.690(5) ? b = 91.593(5), Z = 4, V = 1877.9(10) 3, Dc = 1.459 g/cm3, F(000) = 856, m(MoKa) = 0.324 mm-1, R = 0.0690 and wR = 0.1368 for 3301 observed reflections (I > 2s(I)). The N(1)H…N(3) and N(2)H…O(4) hydrogen bonds can be observed. In the molecule the phenyl plane(I), pyrimi- din-2-yl-urea bridge plane(Ⅱ) and ester plane(Ⅲ) form three conjugated systems.展开更多
文摘Amino acid benzyl ester p-toluenesulfonic acids were synthesized under microwave irradiation condition by reaction of four amino acids with benzyl alcohol and p-toluenesulfonic acid,and then reacted with the N-phthaloyl-L-glutamic anhydride to yield compound 3a-d,hydrogenised and treated with NH3(g) to obtain the target compounds—thalidomide ammonium salt derivatives.The microwave-assisted method was used to synthesis the thalidomide amino acid benzyl ester p-tolunensulfonic acid,the reaction time was brought down with improved yield as compared with conventional heating method.The structures were comfirmed by MS,1H-NMR and elemental analysis.
基金The project was supported by the National Natural Science Foundation of China (20372021) and Natural Science Foundation of Hunan Province (03JJY3018)
文摘The title compound 2-[(4-methoxy-6-methylthio-2-pyrimidinyl)aminocarbonyl- aminosulfonyl]benzoic acid methyl ester (C15H16N4O6S2, Mr = 412.44) was obtained by the reaction of (4-methoxy-6-methylthio-2-pyrimidinyl)amine with 2-methoxylcarbonylbenzene-sulfonylisocya- nate. The crystal is of monoclinic, space group P21/c with a =11.169(3), b = 9.508(3), c = 17.690(5) ? b = 91.593(5), Z = 4, V = 1877.9(10) 3, Dc = 1.459 g/cm3, F(000) = 856, m(MoKa) = 0.324 mm-1, R = 0.0690 and wR = 0.1368 for 3301 observed reflections (I > 2s(I)). The N(1)H…N(3) and N(2)H…O(4) hydrogen bonds can be observed. In the molecule the phenyl plane(I), pyrimi- din-2-yl-urea bridge plane(Ⅱ) and ester plane(Ⅲ) form three conjugated systems.