1,5-苯并硫氮杂-α,α-二甲基-β-内酰胺衍生物的合成、表征及晶体结构

Synthesis and Crystal Structure of α,α-Dimethyl-β-lactam Derivatives of 1,5-Benzothiazepines

利用异丁酸乙酯、异丁酸异丙酯、异丁酸薄荷醇酯和LDA作用形成烯醇锂盐 ,然后和 1,5 苯并硫氮杂反应 ,得到了 6个新的 1,5 苯并硫氮杂 α ,α 二甲基 β 内酰胺衍生物 .通过元素分析、红外光谱、核磁共振氢谱和质谱对其结构进行了表征 .用X射线单晶衍射测定了 1a的晶体结构 .晶体为三斜晶系 ,P1- 空间群 ,晶胞参数为 :a =0 92 99( 3 )nm ,b =1 0 13 4( 3 )nm ,c =1 2 45 5 ( 4 )nm ,α =98 45 7( 5 )° ,β =10 6 14 3 ( 5 )° ,γ =10 3 843 ( 5 )° ,V =1 0 65 7( 6)nm3 ,Z =2 ,Dc=1 2 95Mg/m3 ,F( 0 0 0 ) =44 0 ,μ =0 175mm-1,R1=0 0 40 6,wR2 =0 10 64 .

The α,α-dimethyl-β-lactam derivatives of 1,5-benzothiazepines were synthesized by the reaction of simple lithium ester enolates with 1,5-benzothiazepines. Their structure were characterized by elemental analysis, IR, 1H NMR and MS spectra. The crystal structure was determined by single-crystal X-ray diffraction analysis. The crystal of 1a belongs to triclinic system, space group P1-, unit cell dimensions: a=0.9299(3) nm, b=1.0134(3) nm, c=1.2455(4) nm, α= 98.457(5)°, β=106.143(5)°, γ= 103.843(5)°, V=1.0657(6) nm3, Z=2, D c=1.295 Mg/m3, F(000)=440, μ=0.175 mm -1, R 1=0.0406, wR 2=0.1064.