Potassium Hydroxide → 3-(2-Ethylhexanoyloxy)-5,5-dimethyl-2-(2',5'-dimethylphenyl)-2-cyclohexenone

HRID 65285

反応式

HRID 65285 の反応式
[CH3:1][C:2]1[CH:7]=[CH:6][C:5]([CH3:8])=[CH:4][C:3]=1[CH:9]1[C:14](=[O:15])[CH2:13][C:12]([CH3:17])([CH3:16])[CH2:11][C:10]1=[O:18].[OH-].[K+].[CH2:21]([CH:23]([CH2:27][CH2:28][CH2:29][CH3:30])[C:24](Cl)=[O:25])[CH3:22]>C1C=CC=CC=1.C1CC2OCCOCCOC3C(OCCOCCOC2CC1)CCCC3.CCOCC>[CH2:21]([CH:23]([CH2:27][CH2:28][CH2:29][CH3:30])[C:24]([O:18][C:10]1[CH2:11][C:12]([CH3:16])([CH3:17])[CH2:13][C:14](=[O:15])[C:9]=1[C:3]1[CH:4]=[C:5]([CH3:8])[CH:6]=[CH:7][C:2]=1[CH3:1])=[O:25])[CH3:22]

参加物

7

実験手順

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.

後処理

  1. customwas prepared
  2. temperaturethe reaction mixture refluxed for 12 hrs
  3. wash50 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. dry with materialThe ether solution was dried

出典と根拠

ORDレコード
ord-34b48e88f482444b8bff393b770af19f
出典データセット
uspto-grants-1986_09
特許番号
US04613617

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