HCID 2724269, compound → HCID 18510150, compound

Temperature

30 °C

To a glass autoclave liner is added 249 g of 5,7-dimethyl-3,5,9-decatrien-2-one, 2.2 g of 5% rutheniumon carbon and 200 ml of methanol. The glass liner is sealed inside a 3 L, stainless steel, rocking autoclave and the autoclave purged once with 250 psig N2, once with 250 psig H2 and then charged with 500 psig H2. With mixing, the reaction mixture is heated. At about 75° C., the reaction initiates and begins consuming H2 and exotherms to 170° C. In 10 minutes, the temperature has dropped to 115-120° C. and the pressure dropped to 270 psig. The autoclave is boosted to 1000 psig with H2, mixed at 110-115° C. for an additional 7 hours and 15 minutes then cooled to 30° C. The reaction mixture is removed from autoclave, filtered to remove catalyst and concentrated by evaporation of methanol under vacuum to yield 225.8 g of 5,7-dimethyl-2-decanol.

1. customthe autoclave purged once with 250 psig N2, once with 250 psig H2
2. additioncharged with 500 psig H2
3. additionWith mixing
4. temperaturethe reaction mixture is heated
5. customAt about 75° C., the reaction initiates
6. custombegins consuming H2
7. customexotherms to 170° C
8. additionthe temperature has dropped to 115-120° C.
9. additionthe pressure dropped to 270 psig
10. additionmixed at 110-115° C. for an additional 7 hours and 15 minutes
11. customThe reaction mixture is removed from autoclave
12. filtrationfiltered
13. customto remove catalyst
14. concentrationconcentrated by evaporation of methanol under vacuum

ORD record

ord-42a3b6b265d64f028dc526ff96af4cc4

Source dataset

uspto-grants-2003_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06506717B1