(1R,2S,5R,8S,9R,10S)-8-甲基-4-氮杂-5-苯基-7-氧杂四环[8.2.1.0^(2,9).0(~4,8)]十三-11-烯-3-酮的合成和晶体结构
Synthesis and Crystal Structure of(1R,2S,5R,8S,9R,10S)- 8-Methyl-4-aza-5-phenyl-7-oxatetracyclo[8.2.1.0^(2,9).0^(4,8)]-11-en-3-one
摘要
为确定内型降冰片烯酰亚胺与甲基格氏试剂反应所得加成产物的结构,合成了标题化合物(C18H19NO2)。其结构通过单晶X-射线衍射分析确定,该晶体属正交晶系,空间群为P212121,a = 6.293(1),b = 14.342(3),c = 16.357(3) 牛琕 = 1476.2(5) ?,Z = 4,Dc = 1.266 g/cm3, (MoKa) = 0.082mm-1,F(000) = 600。晶体结构用直接法解出,最终的偏离因子为R = 0.0535,wR = 0.988。由此晶体结构可确定加成产物为标题化合物,并由1H-NMR数据推测另一加成产物的结构。
The title compound (C8H19NO2, Mr=304.13) was synthesized in view of determining the isomeric structures obtained from the reaction of MeMgI with endo-himic imide. X-Ray crystal structure analysis showed that the crystal of one isomer is of orthorhombic, space group P212121 with a = 6.2936(1), b = 14.342(3), c = 16.357(3) ? V = 1476.2(5) ?, Z = 4 and Dc = 1.266 g/cm3. The structure was solved by direct methods. The final R = 0.0535 and wR = 0.988. The unambiguous determination of the structure of the title compound allowed to deduce the structures of other isomers. Present work will found the basis for the development of fused 2-pyrrolidinones as new chiral auxiliaries.
基金
国家自然科学基金资助项目
教育部博士点基金
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