Ethylene → Ethene;oct-1-ene

Participants

Reaction Conditions

Reaction Steps

Under a nitrogen atmosphere, a 500 mL autoclave was charged with hexane (250 mL), triisobutylaluminum (0.2 mL of a 25.2 wt % solution in heptane diluted with toluene (5 mL)) and 1-octene (18 mL, 115 mmol). The autoclave was stirred at ca. 1500 rpm, heated to 140.1° C. (P=75.7 psig) then pressurized with ethylene to 265.6±1 psig. Ethylene flow into the reactor was allowed during the copolymerization. A solution of precatalyst (40-50 μmol), PhNMe2H+ B(C6F5)4− (1 equiv.) and toluene (100 mL) was added to the stirred mixture over 30 min. at a variable rate sufficient to obtain 12-15 g isolated copolymer with an exotherm of less than 1.5° C., typically less than 1° C. The polymer was precipitated with 2-propanol (1.5 L), isolated, then dried under vacuum at 80° C. See Table below.

Provenance & Evidence