10-Undecen-1-ol → HCID 86594890, compound

Temperature

50 °C

900 ml of toluene was introduced into a 1-L glass polymerizer purged with nitrogen, and while an ethylene gas (100 L/h) was circulated, 5.0 ml (5.0 mmol) of stock solution (1.0 M toluene solution) of triethyl aluminum and 0.80 ml (4.0 mmol) of 10-undecen-1-ol were added thereto, and the mixture was stirred at 50° C. for 5 minutes. 17.6 mg of metallocene compound represented by the above formula (XXI) was introduced into another 20-ml Schlenk flask purged with nitrogen, and 1.14 ml of toluene solution of methyl aluminoxane (MAO) (A1=1.37 M) was added thereto and stirred for about 10 seconds, and the resulting solution was added to the polymerization solution. While an ethylene gas was circulated at 100 L/h, the mixture was stirred at 50° C. for 3 minutes (600 rpm). The reaction was terminated with isobutyl alcohol (15 ml) and conc. hydrochloric acid (2 ml), and the reaction solution was poured into 2 L of methanol to precipitate a polymer. The reaction solution was stirred overnight, and the polymer was filtered with a glass filter and then dried at 80° C. under reduced conditions at 10 Torr for 10 hours to give 10.09 g ethylene/10-undecen-1-ol copolymer. As a result of analysis by gel permeation chromatography (GPC), the molecular weight of the polymer was 109300 in terms of polyethylene-equivalent weight-average molecular weight (Mw), and the molecular weight distribution (Mw/Mn) was 3.04. From 1H-NMR measurement results, the content of the comonomer (10-undecen-1-ol) introduced was 0.78 mol-%.

1. custompurged with nitrogen
2. additionwas introduced into another 20-ml Schlenk flask
3. custompurged with nitrogen, and 1.14 ml of toluene solution of methyl aluminoxane (MAO) (A1=1.37 M)
4. additionwas added
5. stirringstirred for about 10 seconds
6. additionthe resulting solution was added to the polymerization solution
7. stirringthe mixture was stirred at 50° C. for 3 minutes (600 rpm)
8. customThe reaction was terminated with isobutyl alcohol (15 ml) and conc. hydrochloric acid (2 ml)
9. additionthe reaction solution was poured into 2 L of methanol
10. customto precipitate a polymer
11. stirringThe reaction solution was stirred overnight
12. filtrationthe polymer was filtered with a glass
13. filtrationfilter
14. customdried at 80° C. under reduced conditions at 10 Torr for 10 hours

ORD record

ord-3eb067051d5f4202a15d73be36590051

Source dataset

uspto-grants-2010_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07795347B2