对甲苯磺酰甘氨酸甲基酯的合成及晶体结构

SYNTHESIS,CRYSTAL STRUCTURE OF METHYL-p- TOLYSULFONYL-GLYCINE

在稀土离子存在条件下 ,对甲苯磺酰甘氨酸与甲醇反应得到对甲苯磺酰甘氨酸甲脂 (Ts Gly HMe) ,并用 X射线衍射测定了其晶体结构 ,化合物属三斜晶系 ,空间群为 P1 - ,分子式为 C1 0 H1 3NO4 S,Mr=2 43 .2 7,晶胞参数 :a=0 .60 2 66(1 0 ) nm,b=0 .70 2 97(1 2 ) nm,c=1 .3 948(2 ) nm;α=83 .647(4 )°,β=80 .93 1 (4 )°,γ=84.3 88(3 )°,V=0 .5 780 1 (1 7) nm3,Z=2 ,Dc=1 .3 98g/ cm3,R1 =0 .0 5 49,w R2 =0 .1 661 .分子在晶胞中是以一种比较伸展的“V”字型方式存在 ,两个化合物分子通过常规氢键形成二聚体 ,二聚体单元以非常规氢键连接成二维层状结构 .同时 ,还改进了对甲苯磺酰氯和对甲苯磺酰甘氨酸的合成方法 .

The title compound,methyl-p-tolysulfonyl-glycine (TsGlyHMe) has been synthesized from the reaction ofp-tolysulfonyl-glycine with solvent molecule of methanol in the presence of rare earth ion.The structure has been determined by X-ray diffraction method.The crystal crystallize in triclinic system,space groupP 1-with C 10H 13NO 4S,Mr=243.27,cell parameters:a=0.60266(10)nm,b= 0.70297(12)nm,c=1.3948(2)nm,α=83.647(4)°,β=80.931(4)°,γ=84.388(3)°,V=0.57801(17)nm3,Z=2,D c=1.398g/cm3,R 1=0.0549,wR 2=0.1661.The molecule exists in the crytal in a form of 'V' model.Two molecules are joined to give a dimer by classical hydrogen bond,and the connection of the dimers via the unclassical hydrogen bond provides a 2-D network.The improved methods for the syntheses of tolylsulfonyl chloride and N-p-tolysulfonyl amino acids have been described in this work.