반응 #93563

ord-34b48e88f482444b8bff393b770af19f

반응 조건

상세 조건
See reaction.notes.procedure_details.

후처리

  1. 1
    기타was prepared
  2. 2
    온도the reaction mixture refluxed for 12 hrs
  3. 3
    세척50 ml of water, washed three times with 0.25N NaOH, two times with water, two times with 6N HCl, and one more with water
  4. 4
    건조The ether solution was dried

실험 절차

A suspension of 1.50 g (6.14 mmol) of 2-(2',5'-dimethylphenyl)-5,5-dimethyl-1,3-cyclohexanedione in 15 ml of dry benzene was prepared and 0.49 g (7.37 mmol) of 85% powered potassium hydroxide was added, followed by 1 drop of dicyclohexyl-18-crown-6-ether. After stirring for 30 minutes, 1.20 (7.37 mmol) of 2-ethylhexanoyl chloride was added, and the reaction mixture refluxed for 12 hrs. The reaction mixture was cooled to room temperature, taken up in 150 ml ether and 50 ml of water, washed three times with 0.25N NaOH, two times with water, two times with 6N HCl, and one more with water. The ether solution was dried and stripped to leave 2.10 g (92% yield) of 3-(2-ethylhexanoyloxy)-5,5-dimethyl-2-(2',5'-dimethylphenyl)-2-cyclohexenone as a clear, colorless oil.

출처

DOI: 10.6084/m9.figshare.5104873.v1특허: US04613617uspto-grants-1986_09