PREPARATION OF NEW PHOSPHORANES (C6H5)2P(O) NHC6F5 AND C6H5P (O)(NHC6F5)2, 1,3-BIS(PENTAFLUOROPHENYL)-2,4-DIPHENYL-1,3,2,4-DIAZADIPHOSPHETIDINE (C6H5PNC6F5)2, AND 1,3-BIS (2-FLUOROPHENYL)-2,4-DIPHENYL-2,4-DIOXO-1,3,2,4-DIAZADIPHOSPHETIDINE (C6H5P (O) NC6H4F)2

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作者
ALAM, K [1 ]
SCOTT, B [1 ]
KIRCHMEIER, RL [1 ]
SHREEVE, JM [1 ]
机构
[1] WASHINGTON STATE UNIV,DEPT CHEM,PULLMAN,WA 99164
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中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Reactions of (C6H5)2P(O)Cl and C6H5P(O)Cl2 with C6F5NH2 yielded the new phosphoranes (C6H5)2P(O)NHC6F5, 1, and C6H5P(O) (NHC6F5)2, 2. When C6H5P(O)Cl2 was reacted with 2-fluoroaniline, the 2,4-dioxo-1,3,2,4-diazadiphosphetidine [C6H5P(O)NC6FH4]2, 3, formed, while with C6H5PCl2, C6F5NH2 gave the new cis-1,3,2,4-diazadiphosphetidine [C6H5PNC6F5]2, 4. Compounds 1, 2, 3, and 4 have been characterized by spectral data (H-1, F-19 and P-31 NMR, IR and MS) and elemental analysis. In addition, 1 has been characterized by single crystal X-ray crystallographic analysis. Lattice parameters and space group information are as follows: a = 9.958(2)angstrom, b = 5.201-(2)angstrom, c = 31.603(6)angstrom, beta = 94.82(2)angstrom, monoclinic, P2(1)/n, Z = 4. The structure was solved and refined by direct methods to R = 0.0789 and R(W) = 0.0936 for 2577 independent reflections. The molecule has both P and N with distorted tetrahedral coordination and has an approximate C2 symmetry axis.
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页码:847 / 854
页数:8
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