Diethyl Ether → 4-Methyl-2-methylene valeric acid

The crude product, ethyl 4-methyl-2-methylenepentanoate containing some ether, was dissolved in absolute ethanol (250 mL) and treated with acetonitrile (250 mL), 1 M LiOH (9.7 g in 250 mL of water, 0.23 mol). After stirring overnight, the organic solvents were evaporated under reduced pressure and the aqueous residue was extracted with ethyl acetate (2×150 mL). The combined extracts were washed with brine, dried over MgSO4 and concentrated under reduced pressure to afford 10.5 g of 4-methyl-2-methylenepentanoic acid as a colorless oil.

1. customthe organic solvents were evaporated under reduced pressure
2. extractionthe aqueous residue was extracted with ethyl acetate (2×150 mL)
3. washThe combined extracts were washed with brine
4. dry with materialdried over MgSO4
5. concentrationconcentrated under reduced pressure

ORD-Eintrag

ord-62d9ff7ab6f24e1fbe3cf50d789ceaa5

Quelldatensatz

uspto-grants-2000_01

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US06013792