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红霉素A6,9-亚胺醚的合成及晶体结构测定
Synthesis and Crystal Structure of Erythromycin A 6,9-Imino Ether
【摘要】 通过红霉素A 9(E) 肟 ( 1)的Beckmann重排合成了红霉素A 6,9 亚胺醚 ( 2 ) ,并对 2进行了波谱表征 .红霉素A 6,9 亚胺醚 ( 2 )的X射线衍射单晶结构测定表明 ,其结构为正交晶系 ,P2 12 12 1空间群 ,晶胞参数 :a =1 0 64 6( 2 )nm ,b =1 7896( 4 )nm ,c =2 3 75 5 ( 5 )nm ;α =β =γ =90 0 0 ( 0 )° ,V =4 5 2 5 7( 16)nm3 ,Dc=1 187g/cm3 ,Z =4,F( 0 0 0 ) =1776,μ =0 0 91mm-1,R1=0 0 3 99,wR2 =0 0 482
【Abstract】 Beckmann rearrangement of erythromycin A 9(E)-oxime (1) generates erythromycin A 6,9-imino ether (2) which has been characterized by NMR, IR, MS and elemental analysis. Crystal structure of 2 was determined by X-ray single crystal diffraction study. The crystal of erythromycin A 6,9-imino ether belongs to orthorhombic system and space group P2 12 12 1 with parameters: a=1 0646(2) nm, b=1 7896(4) nm, c=2 3755(5) nm, α=β= γ=90 00(0)°, V=4 5257(16) nm3, D c=1 187 g/cm3, Z=4, F(000)=1776, μ=0 091 mm -1, R 1=0 0399, wR 2=0 0482.
【Key words】 erythromycin A 6; 9-imino ether; Beckmann rearrangement; identification; crystal structure;
- 【文献出处】 有机化学 ,Chinese Journal of Organic Chemistry , 编辑部邮箱 ,2003年08期
- 【分类号】TQ465
- 【被引频次】9
- 【下载频次】269