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N-甲基-4-硝基苄甲基磺酰胺是合成舒马曲坦和纳拉曲坦的关键中间体。以氯化苄为原料,经硝化、磺酰化、氯化、甲胺化四步反应得到标题化合物,纯度>99%,总收率为67.1%。以无水乙醇为溶剂.经溶剂挥发得到目标产物单晶,并通过熔点、元素分析、MS、1H-NMR和X射线单晶衍射仪确定了结构对产物进行了谱学表征和晶体结构分析。该晶体属于正交晶系.Pca21空间群,晶胞参数:a=15.062(3)nm,b=11.882(2)nm,c=11.287(2)nm.α=90.00°,β=90.00°,γ=90.00°,v=2.0200(7)nm3,Dx=1.514g/cm3,Z=4,F(000)=960,μ=0.317mm-1,S=1.003,R=0.0688,wR=0.169。
N-methyl-4-nitrobenzyl methanesulfonamide is the key intermediate for the synthesis of sumatriptan and naratriptan. Benzyl chloride as raw material, the nitration, sulfonylation, chlorination, methylamine four-step reaction to give the title compound, purity> 99%, the total yield of 67.1%. The product was identified by melting point, elemental analysis, MS, 1H-NMR and X-ray single crystal diffractometer. The structure of the product was characterized by spectral analysis and crystal structure analysis. The crystal belongs to the orthorhombic system. The Pca21 space group has unit cell parameters of a = 15.062 (3) nm, b = 11.882 (2) nm and c = 11.287 (2) nm. γ = 90.00 °, v = 2.0200 (7) nm3, Dx = 1.514 g / cm3, Z = 4, F (000) = 960, μ = 0.317 mm-1, S = 1.003, R = 0.0688, wR = 0.169.