(+)-O-萘基环状磷酰二胺酯的合成、晶体结构及绝对构型

合成了目标化合物(+)-O-萘基环状磷酰二胺酯,其结构由¹HNMR,³¹PNMR及元素分析确定,并在273K下进行了X射线衍射晶体结构分析.该化合物晶体属正交晶系,P2₁2₁2₁空间群,晶胞参数a=1.0028(4)nm,b=1.1406(4)nm,c=2.4455(8)nm,V=2.7971(18)nm₃,Z=4,Dc=1.212g/cm³,F(000)=1088,μ=0.129mm^-1.晶体的结构收敛最终偏离因子R和wR分别为0.0585和0.0827.Flackx参数为0.03(12).目标化合物中磷原子的绝对构型为S.     

Synthesis, Crystal Structure and AbsoluteConfiguration of （＋）-O-Phenyl Cyclophosphorodiamidate

The title compound, ( )-O-phenyl cyclophosphorodiamidate (C28H33N202P, Mr=460.53), has been synthesized and characterized by 31p NMR, 1H NMR and elemental analysis. X-ray diffraction analysis at 273(2) K indicates that it belongs to orthorhombic system, space group P212121 with a=11.518(4), b=13.449(4), c=16.539(5)A, V=2562(1)A3, Z=4, Dc=1.194g/cm3, F(000)=984 and μ(MoKα)=0.134mm-l. The structure parameters were refined by full-matrix least-squares on F2 to R=0.0459 and wR=0.0640. The flack χ parameter is 0.03(10), and the absolute configuration of the phosphorus atom in the title compound is S.