21-11-2013 дата публикации
Номер: US20130310590A1
Compounds 1,3,4-(SiMe)(CF)(alkyl)CHare made using a simplified synthetic strategy which is readily scalable. On reaction with a suitable transition metal species, a 1,3,4-(SiMe)(CF)(alkyl)CHmolecule provides an organotransition metal complex comprising a 1,2-(CF)(alkyl) substituted cyclopentadienyl ligand, which is active toward olefin polymerization. 1. A method for making the compound 1 ,3 ,4-(SiMe)(CF)(R)CHwithout isolating intermediates , said method comprising the following steps:{'sub': 6', '6', '5', '5', '6', '5', '5', '4, 'sup': 1', '2', '1', '1', '2, 'Step 1) in the presence of an ethereal solvent, combining perfluorobenzene CF, a metal cyclopentadienide [M][CH] and a first base MBto form a first reaction mixture comprising [M/M][(CF)CH];'}{'sub': 3', '3', '6', '5', '5', '4, 'Step 2) combining at least 2 molar equivalents of ClSiMewith said first reaction mixture to give a second reaction mixture comprising 1,3-(SiMe)(CF)CH;'}{'sup': 3', '2', '1', '2', '3, 'sub': 3', '6', '5', '5', '3, 'Step 3) combining a second base MBwith said second reaction mixture to give a third reaction mixture comprising [M/M/M][1,3-(SiMe)(CF)CH];'}{'sub': 3', '6', '5', '5', '3, 'claim-text': {'sup': 1', '2', '3', '+', '+', '+', '1', '2, 'wherein M, M, Mare the same or different metal selected from the group consisting of Li, Na and K; Band Bare the same or different base selected from the group consisting of hydride, alkylide, amide and alkoxide; R is a primary or secondary alkyl group; and X is a halide group or a sulfonate group.'}, 'Step 4) combining a compound RX with said third mixture to give a fourth reaction mixture comprising 1,3,4-(SiMe)(CF)(R)CH;'}2. The method of wherein approximately equimolar amounts of CF claim 1 , [Na][CH] and NaH are combined in step 1.3. The method of wherein CFis combined with approximately 2 molar equivalents of [Na][CH] in step 1.4. The method of wherein CFis added slowly over at least 30 min to approximately 2 molar equivalents of [Na][CH] in ...
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