Reaktion #979299
ord-ae98f0a75b9f4b9ba79e7eab29862792
Reaktionsgleichung
Edukte
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
60°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1workup.STIRRINGthe mixture was stirred
- 2Waschenthe organic layer was washed with water
- 3Trocknendried over magnesium sulfate
- 4EinengenThe organic layer was concentrated and to the residue
- 5workup.ADDITIONwere added dichloromethane and diisopropyl ether
- 6FiltrationThe deposited crystals were collected by filtration
Vorschrift
Compound 67a (82 mg, 0.20 mmol) obtained in Example 67 was dissolved in tetrahydrofuran (1 mL), to the solution was added a 1 mol/L solution (2 mL) of ethyl magnesium bromide in tetrahydrofuran, and the mixture was stirred at 60° C. for 1 hour. To the reaction mixture was added water and the mixture was stirred. Ethyl acetate was added to the mixture and the organic layer was washed with water and dried over magnesium sulfate. The organic layer was concentrated and to the residue were added dichloromethane and diisopropyl ether. The deposited crystals were collected by filtration to obtain the title compound (40 mg, 58%) as a white solid.