Reaktionsgleichung
[CH2:1]=[C:2]([CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]([O:5]CC)=[O:4].[OH-].[K+]>CO>[CH2:1]=[C:2]([CH2:8][C:9]1[CH:14]=[CH:13][CH:12]=[CH:11][CH:10]=1)[C:3]([OH:5])=[O:4]Komponenten
4
Edukt 2
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
The ethyl α-methylenebenzenepropanoate of Step 8 (4.6 g, 24.3 mmol) was dissolved in methanol (12 mL) and then reacted with 2N potassium hydroxide (24 mL) solution. The mixture was stirred at room temperature for 4 hours and concentrated by evaporation. The residue was diluted with water and washed with ether. The aqueous layer was acidified to pH 2 with 1N HCl, and then extracted with ethyl acetate. The extracts were dried (MgSO4) and evaporated to give the title compound as colorless oil (2.8 g, 66% yield). 1H NMR: 300MHz spectrum consistent with proposed structure.
Aufarbeitung
- concentrationconcentrated by evaporation
- additionThe residue was diluted with water
- washwashed with ether
- extractionextracted with ethyl acetate
- dry with materialThe extracts were dried (MgSO4)
- customevaporated
Quellen und Nachweise
- ORD-Eintrag
- ord-c2667c1c1f0b427fbd77fc2f264f3da1
- Quelldatensatz
- uspto-grants-1995_05
- Patentnummer
- US05414018
Verknüpfte Notizen
Wird geladen…