Reaktion #514592
ord-9304d89c4e324764996841c307a765a8
Reaktionsgleichung
Reagenzien
Keine
Lösungsmittel
Reaktionsbedingungen
Temperatur
45°CELSIUS
Detaillierte Bedingungen
See reaction.notes.procedure_details.
Aufarbeitung
- 1Sonstigekept at 35° C.
- 2workup.ADDITIONAfter addition
- 3TemperaturThe reaction was cooled
- 4ExtraktionThe product was extracted with EtOAc
- 5ExtraktionThe organic layer was extracted with 1 N NaOH
- 6Sonstigeto produce a white precipitate that
- 7Filtrationwas collected by filtration
- 8Waschenwashed with water
- 9Sonstigedried
Vorschrift
To a mixture of AlCl3 (13 g, 97.5 mmol, 1.0 equiv) in benzene (100 mL) kept at 35° C., was added 1-cyclohexenecarboxylic acid (5 g, 39.7 mmol, 0.41 equiv) dropwise. After addition was complete, the reaction solution was heated to 70° C. for 1 h and 45° C. overnight. The reaction was cooled, and 200 mL of 1 N HCl was slowly added. The product was extracted with EtOAc. The organic layer was extracted with 1 N NaOH and the aqueous layer was acidified with concentrated HCl to produce a white precipitate that was collected by filtration, washed with water and dried to give the titled compound as a white solid (3.1 g, 38%) which was used without further purification.