Reaktion #64722
ord-0208c64273a84e8e8c4fda96508a2f39
Reaktionsgleichung
Reagenzien
Lösungsmittel
Reaktionsbedingungen
Aufarbeitung
- 1workup.ADDITIONwas added
- 2TemperaturThe mixture was heated
- 3Temperaturunder reflux for 3.5 hours
- 4Filtrationinsoluble substances were filtered off
- 5EinengenThe filtrate was concentrated
- 6Extraktionthe residue was subjected to extraction with the addition of water and ethyl acetate
- 7SonstigeThe organic layer was separated
- 8Extraktionthe aqueous layer was then extracted with ethyl acetate
- 9Trocknendried over anhydrous magnesium sulfate
- 10SonstigeThe solvent was evaporated off under reduced pressure
- 11Sonstigethe residue was purified by silica gel chromatography
Vorschrift
In 50 ml of tetrahydrofuran were dissolved 1.5 g of 1-(2-chlorophenyl)piperazine and 5 ml of triethylamine, and 3.4 g of 2-[bis(4-hydroxyphenyl)methyl]benzylbromide was added thereto. The mixture was heated under reflux for 3.5 hours, and then insoluble substances were filtered off. The filtrate was concentrated, and the residue was subjected to extraction with the addition of water and ethyl acetate. The organic layer was separated, and the aqueous layer was then extracted with ethyl acetate. The organic layers were combined and then dried over anhydrous magnesium sulfate. The solvent was evaporated off under reduced pressure, and the residue was purified by silica gel chromatography to afford 0.54 g of the desired compound (Compound 89).