(R)-2-羟甲基-1-氮杂-4-硫杂螺[4.5]癸烷的合成及晶体结构  

Synthesis and Crystal Structure of (R)-2-Hydroxymethyl-1- aza-4-thiaspiro[4.5]decane

作　　者：王辉[1] 裴伟伟[1] 章士伟[1] 孙国斌[1] 

机构地区：[1]北京大学化学与分子工程学院,北京100871

出　　处：《北京大学学报（自然科学版）》2004年第6期849-854,共6页Acta Scientiarum Naturalium Universitatis Pekinensis

摘　　要：合成了标题化合物C9H17NOS ,它的晶体结构已经用X 射线单晶衍射法测定。晶体属正交晶系 ,P2 12 12 1空间群 ,晶胞参数a =0 6 70 4 (1)nm ,b =0 816 7(2 )nm ,c =1 82 6 7(4 )nm ,V =1 0 0 0 0 (3)nm3 ,Z =4 ,Mr=187 30 ,Dc =1 2 4 4g cm3 ,F(0 0 0 ) =4 0 8,μ(MoKα) =0 2 79mm-1。晶体结构用直接法解出 ,经全矩阵最小二乘法对原子参数进行修正 ,最终的偏离因子为R =0 0 2 95 ,wR=0 0 6 42。结构测定表明标题化合物是单螺化合物。由C(1)、C(2 )、C(3)、C(4 )、C(5 )和C(6 )构成的六元环取椅型构象 ,由C(1)、S、C(7)、C(8)和N构成的五元环取半椅型构象 ,两个环共用的螺原子C(1)用sp3 杂化轨道与其他原子成键。晶体结构分析表明存在着分子间氢键。The title compound C 9H 17NOS was synthesized and its crystal structure was determined by single crystal X-ray diffraction. The crystal is orthorhombic system, space group P2 12 12 1 with parameters a= 0.670?4 (1)?nm, b= 0.816?7 (2)?nm, c= 1.826?7 (4)?nm, V= 1.000?0 (3)?nm3, Z=4, Mr= 187.30, Dc= 1.244?g/cm3, F(000)=408, μ(MoK α)= 0.279?mm -1. The structure was solved by direct methods and refined by full matrix least squares to the final R= 0.029?5, wR= 0.064?2. X-ray analysis reveals that the compound is a single spiral compound. The six-membered ring which is composed of C (1), C (2), C (3), C (4), C (5), and C (6) is chair conformation. The five-membered ring which is composed of C (1), S, C (7), C (8), and N is half-chair conformation. Crystal structural analysis shows that intermolecular hydrogen bonds occur between hydroxyl group and nitrogen atom.

关 键 词：(R)-2-羟甲基-1-氮杂-4-硫杂螺[4.5]癸烷 合成 晶体结构 手性催化剂 分子间氢键 

分 类 号：O621[理学—有机化学]