In:
Zeitschrift für Naturforschung B, Walter de Gruyter GmbH, Vol. 50, No. 6 ( 1995-6-1), p. 923-930
Kurzfassung:
The reaction of (η 5 -C 5 H 4 SiMe 3 ) 2 TiCl 2 (1) with HO(CH 2 ) n C ≡ CR (2a: n = 1, R = H; 2b: n = 1, R = CH 3 ; 2c: n = 1, R = CH 2 OH ; 3: n = 2, R = H; 4: n = 4, R = H) affords in toluene at 25 °C in the presence of NEt 3 the monoalkyne-ol substituted titanocenes (η 5 -C 5 H 4 SiMe 3 ) 2 Ti(Cl)[O(CH 2 ) n C ≡ CR] (5a: n = 1. R = H; 5b: n = 1, R = CH 3 ; 5c: n = 1, R = C H 2 OH; 6: n = 2, R = H; 7: n = 4. R = H ). Compound 5c reacts with one equivalent of 1 in the presence of NEt 3 to yield (η 5 -C 5 H 4 SiMe 3 ) 2 (Cl)Ti-OCH 2 C ≡ CCH 2 O -Ti(Cl)(η 5 -C 5 H 4 SiMe 3 ) 2 (8). In addition, compound 8 can be synthesized directly by treatment of (η 5 - C 5 H 4 SiMe 3 ) 2 TiCl 2 (1) with 0.5 equivalents of HOCH 9 C≡CCH 2 OH (2c) in the presence of NEt 3 . The reaction of (η 5 -C 5 H 4 SiMe 3 ) 2 Ti(Cl)(OCH 2 C ≡ CCH 3 ) (5b) with Co 2 (CO) 8 (9) yields (η 5 -C 5 H 4 SiMe 3 ) 2 Ti(Cl)[(η 2 -OCH 2 C ≡ CCH 3 )Co 2 (CO) 6 ] (10). Treatment of 5b or 10 with HCl (aq) (11) leads to the formation of (η 5 -C 5 H 4 SiMe 3 ) 2 TiCl 2 (1) and HOCH 2 C ≡ CCH 3 (2b) (reaction of 5b with 11) or (η 5 -C 5 H 4 SiMe 3 ) 2 TiCl 2 (1) and [(η 2 -HOCH 2 C ≡ CCH 3 )Co 2 (CO) 6 ] (12) (reaction of 10 with 11). All compounds have been characterized by analytical and spectroscopic data (IR , 1 H, 13 C NMR, MS) and (η 5 -C 5 H 4 SiMe 3 ) 2 Ti(Cl)(OCH 2 C ≡ CCH 3 ) (5b) by X -ray analysis.
Materialart:
Online-Ressource
ISSN:
1865-7117
,
0932-0776
DOI:
10.1515/znb-1995-0614
Sprache:
Englisch
Verlag:
Walter de Gruyter GmbH
Publikationsdatum:
1995
ZDB Id:
2078109-X
ZDB Id:
124635-5
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