hydrogenchloride; tetrakis(triphenylphosphine) palladium(0) in tetrahydrofuran T=50°C; 1.5 h; Inert atmosphere;

tetrakis(triphenylphosphine) palladium(0) in tetrahydrofuran T=60°C; 1 h; Product distribution / selectivity;

tetrakis(triphenylphosphine) palladium(0) in tetrahydrofuran T=80°C; 16 h; Product distribution / selectivity;

in hexane; benzene a mixt. of Cp2ZrHCl and 1-octene in benzene was stirred for ca. 2 h at room temp. under N2, a soln. of anhyd. SnCl4 in n-hexane was added dropwise (Cp2ZrHCl/SnCl4 ratio 2:1), stirred for a further 1 h 30 min; hexane was added, ppt. of Cp2ZrCl2 was filtered off, filtrate was concd., residue extd. with hexane, exts. were combined, concd., dild. with methanol; (octyl)SnCl3 content was detd. by titrn. with 0.02 M EDTA;

tert-butyl methyl ether; tin(IV) chloride T=50°C; 0.75 h; Product distribution / selectivity;

in hexane; benzene a mixt. of Cp2ZrHCl and 3-octene in benzene was stirred for ca. 2 h at room temp. under N2, a soln. of anhyd. SnCl4 in n-hexane was added dropwise (Cp2ZrHCl/SnCl4 ratio 2:1), stirred for a further 1 h 30 min; hexane was added, ppt. of Cp2ZrCl2 was filtered off, filtrate was concd., residue extd. with hexane, exts. were combined, concd., dild. with methanol; (octyl)SnCl3 content was detd. by titrn. with 0.02 M EDTA;

in hexane; benzene a mixt. of Cp2ZrHCl and 2-octene in benzene was stirred for ca. 2 h at room temp. under N2, a soln. of anhyd. SnCl4 in n-hexane was added dropwise (Cp2ZrHCl/SnCl4 ratio 2:1), stirred for a further 1 h 30 min; hexane was added, ppt. of Cp2ZrCl2 was filtered off, filtrate was concd., residue extd. with hexane, exts. were combined, concd., dild. with methanol; (octyl)SnCl3 content was detd. by titrn. with 0.02 M EDTA;

in hexane; benzene a mixt. of Cp2ZrHCl and 1-octene in benzene was stirred for ca. 2 h at room temp. under N2, a soln. of anhyd. SnCl4 in n-hexane was added dropwise (Cp2ZrHCl/SnCl4 ratio 4:1), stirred for a further 1 h 30 min; hexane was added, ppt. of Cp2ZrCl2 was filtered off, filtrate concd., residue extd. with hexane, exts. concd., dild. with methanol; (octyl)SnCl3 content was detd. by titrn. with EDTA, yield of (octyl)2SnCl2 was estimated by conversion into (octyl)2SnO;

1: anhydrous butyl ether View Scheme

1: 2,2,4-trimethylpentane View Scheme