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Metal Imido Complexes (M=Ti, W) Containing 2‐(Dimethylaminomethyl)pyrrole: Synthesis and the Crystal Structures of Bu t N=TiCIPy 2 [2‐Me 2 NCH 2 (C 4 H 3 N)] and PhN=WCl 3 [2‐Me 2 NCH 2 (C 4 H 3 N)]
Author(s) -
Huang JuiHsien,
Chi LiangSheng,
Huang FengMau,
Kuo PeiCheng,
Zhou ChongChin,
Lee GeneHsiang,
Peng ShieMing
Publication year - 2000
Publication title -
journal of the chinese chemical society
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.329
H-Index - 45
eISSN - 2192-6549
pISSN - 0009-4536
DOI - 10.1002/jccs.200000121
Subject(s) - chemistry , monoclinic crystal system , diethyl ether , crystal structure , octahedron , ether , metathesis , medicinal chemistry , hydrolysis , crystallography , stereochemistry , yield (engineering) , lithium (medication) , metal , methylene , organic chemistry , polymerization , medicine , materials science , metallurgy , endocrinology , polymer
A titanium imido complex, Bu t N=TiClPy 2 [2‐Me 2 NCH 2 ‐(C 4 H 3 N)] 1 , was synthesized through metathesis by reacting Bu t N=TiCl 2 Py 3 with lithium 2‐(dimethylaminomethyl) pyrrolate (LLi) in diethyl ether at room temperature. The dark brown red crystals were obtained from a concentrated diethyl ether solution of compound 1 at −20°C and the monoclinic crystal shows a distorted octahedral structure with two pyridines taking trans positions. Hydrolysis Bu t N=TiCl 2 Py 3 with 2,2′‐methylene‐bis(6‐t‐butyl‐4‐methylphenol) (HO∼∼CH 2 ∼∼OH) generates a bis phenoxide titanium complex, (O∼∼CH 2 ∼∼O)TiCl 2 Py 2 , by eliminating one equivalent of Bu t NH 2 . Similarly, the reaction of LH with PhN=WCl 4 (OEt 2 ) in diethyl ether at room temperature generates PhN=WCl 3 (L) 3 , in moderate yield. 3 has been characterized by NMR spectroscopies and X‐ray crystallography.