反应详情

温度

45 °C

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.

1. customkept at 35° C.
2. additionAfter addition
3. temperatureThe reaction was cooled
4. extractionThe product was extracted with EtOAc
5. extractionThe organic layer was extracted with 1 N NaOH
6. customto produce a white precipitate that
7. filtrationwas collected by filtration
8. washwashed with water
9. customdried