Multiple syntheses of (C5Me5)3U

被引:92
作者
Evans, WJ [1 ]
Nyce, GW [1 ]
Forrestal, KJ [1 ]
Ziller, JW [1 ]
机构
[1] Univ Calif Irvine, Dept Chem, Irvine, CA 92697 USA
关键词
D O I
10.1021/om010831t
中图分类号
O61 [无机化学];
学科分类号
070301 ; 081704 ;
摘要
Several new synthetic routes to the sterically crowded (C5Me5)(3)U complex have been developed. (C5Me5)(3)U can be prepared by (a) reaction of [(C5Me5)(2)UH2](2) with tetramethylfulvene, (b) reduction of (C5Me5)(2)Pb with (C5Me5)(2)UH(DMPE), (c) reaction of [(C5Me5)(2)U- (L)](+) (L = THF, DMPE) with K(18-crown-6)(C5Me5), and (d) reaction of [(C5Me5)(2)U][BPh4] with KC5Me5. Reaction of (C5Me5)(2)UH(DMPE) with C8H8 forms the product of the (C5Me5)(3)U/C8H8 reaction, [(C8H8)(C5Me5)U](2)(C8H8). The X-ray crystal structures of the (C5Me5)(2)U-[N(SiMe3)(2)] and [(C5Me5)(2)U][BPh4] precursors used in this study are reported, as well as the convenient synthesis of a new trivalent uranium precursor, (C5Me5)(2)UMe2K.
引用
收藏
页码:1050 / 1055
页数:6
相关论文
共 47 条
[21]   SYNTHESIS AND REACTIVITY OF THE CATIONIC ORGANOSAMARIUM(III) COMPLEX [(C5ME5)2SM(THF)2][BPH4], INCLUDING THE SYNTHESIS AND STRUCTURE OF A METALLOCENE WITH AN ALKOXY-TETHERED C5ME5 RING, (C5ME5)2SM[O(CH2)4C5ME5](THF) [J].
EVANS, WJ ;
ULIBARRI, TA ;
CHAMBERLAIN, LR ;
ZILLER, JW ;
ALVAREZ, D .
ORGANOMETALLICS, 1990, 9 (07) :2124-2130
[22]   Unsolvated lanthanide metallocene cations [(C5Me5)2Ln][BPh4]:: Multiple syntheses, structural characterization, and reactivity including the formation of (C5Me5)3Nd [J].
Evans, WJ ;
Seibel, CA ;
Ziller, JW .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1998, 120 (27) :6745-6752
[23]   Activity of [Sm(C5Me5)(3)] in ethylene polymerization and synthesis of [U(C5Me5)(3)], the first tris(pentamethylcyclopentadienyl) 5f-element complex [J].
Evans, WJ ;
Forrestal, KJ ;
Ziller, JW .
ANGEWANDTE CHEMIE-INTERNATIONAL EDITION IN ENGLISH, 1997, 36 (07) :774-776
[24]   How much steric crowding is possible in tris(η5-pentamethylcyclopentadienyl) complexes?: Synthesis and structure of (C5Me5)3UCl and (C5Me5)3UF1 [J].
Evans, WJ ;
Nyce, GW ;
Johnston, MA ;
Ziller, JW .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 2000, 122 (48) :12019-12020
[25]   SYNTHESIS AND PROPERTIES OF BIS(PENTAMETHYLCYCLOPENTADIENYL) ACTINIDE HYDROCARBYLS AND HYDRIDES - A NEW CLASS OF HIGHLY REACTIVE F-ELEMENT ORGANO-METALLIC COMPOUNDS [J].
FAGAN, PJ ;
MANRIQUEZ, JM ;
MAATTA, EA ;
SEYAM, AM ;
MARKS, TJ .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1981, 103 (22) :6650-6667
[26]   SYNTHESIS AND PROPERTIES OF A NEW CLASS OF HIGHLY REACTIVE TRIVALENT ACTINIDE ORGANO-METALLIC COMPOUNDS - DERIVATIVES OF BIS(PENTAMETHYLCYCLOPENTADIENYL)URANIUM(III) [J].
FAGAN, PJ ;
MANRIQUEZ, JM ;
MARKS, TJ ;
DAY, CS ;
VOLLMER, SH ;
DAY, VW .
ORGANOMETALLICS, 1982, 1 (01) :170-180
[27]  
JUTZI P, 1992, SYNTHESIS-STUTTGART, P1096
[28]   C-H bonds are not elongated by coordination to lanthanide metals:: Single-crystal neutron diffraction structures of (C5Me5)Y(OC6H3tBu2)CH(SiMe3)2 at 20 K and (C5Me5)La{CH(SiMe3)2}2 at 15 K [J].
Klooster, WT ;
Brammer, L ;
Schaverien, CJ ;
Budzelaar, PHM .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1999, 121 (06) :1381-1382
[29]   DIOXYGEN ACTIVATION BY GROUP-4 TRITOX ALKYLS (TRITOX = TERT-BU3CO-) - INSERTION AND OXYGEN ATOM TRANSFER [J].
LUBBEN, TV ;
WOLCZANSKI, PT .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1987, 109 (02) :424-435
[30]   SYNTHESIS, CHEMISTRY, AND SPECTROSCOPY OF SOME TRIS(PENTAHAPTOCYCLOPENTADIENYL)URANIUM(IV) ALKYL AND ARYL COMPOUNDS [J].
MARKS, TJ ;
SEYAM, AM ;
KOLB, JR .
JOURNAL OF THE AMERICAN CHEMICAL SOCIETY, 1973, 95 (17) :5529-5539