Reaktion #1694082
ord-85d273785ce44d13bd1b40815c31a667
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
50°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1TemperaturThis is cooled
- 2Sonstigethe methanol is removed under vacuo
- 3workup.ADDITIONdiluted with 30 ml water
- 4Filtrationfiltered
- 5Extraktionextracted with ethyl acetate
- 6Waschenwashed with water
- 7Trocknendried over magnesium sulfate
- 8Sonstigeevaporated to dryness
- 9Sonstigeto give crystalline product which
Vorschrift
A mixture of 1.6 g of methyl 2-chloro-5a,6,7,8,9,9a-hexahydrodibenzofuran-4-carboxylate in 10 ml of methanol and 20 ml of 1N sodium hydroxide is stirred at 50° C. for 6 hours. This is cooled, the methanol is removed under vacuo, diluted with 30 ml water and filtered. The aqueous solution is acidified with acetic acid, extracted with ethyl acetate, washed with water, dried over magnesium sulfate and evaporated to dryness to give crystalline product which is used directly in the next step.