US 12,479,874 B2
Synthesis of metallocene polymerization catalyst
Charles Carter, Calgary (CA); and Janelle Smiley-Wiens, Calgary (CA)
Assigned to NOVA Chemicals (International) S.A., Fribourg (CH)
Appl. No. 17/440,424
Filed by NOVA CHEMICALS (INTERNATIONAL) S.A., Fribourg (CH)
PCT Filed Mar. 16, 2020, PCT No. PCT/IB2020/052396
§ 371(c)(1), (2) Date Sep. 17, 2021,
PCT Pub. No. WO2020/188473, PCT Pub. Date Sep. 24, 2020.
Claims priority of application No. 3037415 (CA), filed on Mar. 20, 2019.
Prior Publication US 2022/0153771 A1, May 19, 2022
Int. Cl. C07F 17/00 (2006.01)
CPC C07F 17/00 (2013.01) 13 Claims
 
1. A method for making a metallocene (II-Cl2) having the structure,

OG Complex Work Unit Chemistry
the method comprising forming a compound (I) having the structure,

OG Complex Work Unit Chemistry
by combining in a single reaction vessel containing an ether solvent, compounds (i) and (11):

OG Complex Work Unit Chemistry
and
with at least 2 molar equivalents of a metal salt of bis(trimethylsilyl)amide of the formula [M+][N(SiMe3)2−] per total number of moles of the compounds (i) and (ii); to give compound (I); and
reacting in the same reaction vessel compound (I) with a Group IV transition metal chloride of the formula M*Cl4;
wherein:
the method is a one pot method;
R1 and R2 are independently an unsubstituted or substituted alkyl, aryl, or alkenyl group;
R3 is hydrogen, or an unsubstituted or substituted alkyl, aryl, or alkenyl group, or a substituted silyl group;
R4A and R4B are independently a hydrocarbyl group, or hydrogen;
M+ is Li+, Na+, or K+; and
M* is Ti, Zr, or Hf.