2,3,5-Triiodobenzoic acid → 1-Decene

Temperatur

90 °C

A solution of 100 g of purified 1-decene, 1.301 g of a TIBA stock solution (20 mg TIBA/g toluene solution) and 0.445 g of Metallocene A stock solution (1 mg Metallocene A/g toluene solution) was charged into a clean 600 ml autoclave equipped with an agitator, at room temperature. The reactor was then pressurized with 30 psig hydrogen. The mixture was then heated to 90° C. with stirring. A second solution made by adding a) 0.641 g of Activator A stock solution (1 mg Activator A/g toluene solution) and b) 20 g toluene solvent and was added and the reaction temperature was maintained at 90° C. overnight, then cooled down to room temperature, and any reactor pressure was vented. The liquid product was diluted with 50 ml heptane, stirred with 5 g activated alumina for half an hour and filtered to remove solids. The filtrate was analyzed by gas chromatography using an internal standard to obtain the wt % of normal-decane (n-C10) formation from 1-decene hydrogenation, wt % conversion to lubes and wt % lube yield. The lube product was then isolated by flashing the light ends (solvents, unreacted C10 fraction, and any fractions lighter than C30) and distilled at 180° C. under high vacuum (1 millitorr) for two hours to isolate the lube product.

1. customequipped with an agitator, at room temperature
2. additionwas added
3. temperaturethe reaction temperature was maintained at 90° C. overnight
4. temperaturecooled down to room temperature
5. customany reactor pressure was vented
6. stirringstirred with 5 g
7. customfor half an hour
8. filtrationfiltered
9. customto remove solids

ORD-Eintrag

ord-70b03b60d66c4e9c88f474373cab2e3a

Quelldatensatz

uspto-grants-2013_09

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08530712B2