4-Hydroxybenzaldehyde → HCID 178444467, 화합물

HRID 2371348노트

반응식

HRID 2371348 반응식
[OH:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=1.[CH2:10]([C@H:15]1[CH2:20][CH2:19][C@H:18]([CH2:21][CH2:22][CH2:23]Br)[CH2:17][CH2:16]1)[CH2:11][CH2:12][CH2:13][CH3:14].C(=O)([O-])[O-].[K+].[K+].CC(=O)CC>O>[CH2:10]([C@H:15]1[CH2:20][CH2:19][C@H:18]([CH2:21][CH2:22][CH2:23][O:1][C:2]2[CH:9]=[CH:8][C:5]([CH:6]=[O:7])=[CH:4][CH:3]=2)[CH2:17][CH2:16]1)[CH2:11][CH2:12][CH2:13][CH3:14]

참가 물질

6

반응물 4

HCID 1264-HydroxybenzaldehydeHCID 6569Methyl Ethyl KetoneHCID 11430Potassium CarbonateHCID 178444432HCID 178444432, 화합물

생성물 1

HCID 178444467HCID 178444467, 화합물수율 121.9%

시약·촉매·용매 1

HCID 962Water용매

실험 절차

A mixture of 1.9 g of 4-hydroxybenzaldehyde, 5.0 g of 3-(trans-4-pentylcyclohexyl)-1-propyl bromide, 8.3 g of potassium carbonate and 50 ml of butanone was heated under reflux overnight. Subsequently, the cooled reaction mixture was poured into water and extracted three times with 50 ml of diethyl ether each time. The combined organic phases were washed with 500 ml of water, dried over magnesium sulphate, filtered and concentrated. Chromatography of the residue on silica gel with toluene and recrystallization from ethanol gave 6.0 g of pure 4-[3-(trans-4-pentylcyclohexyl)-1-propyloxy]benzaldehyde.

후처리

  1. temperaturewas heated
  2. temperatureunder reflux overnight
  3. customSubsequently, the cooled reaction mixture
  4. extractionextracted three times with 50 ml of diethyl ether each time
  5. washThe combined organic phases were washed with 500 ml of water
  6. dry with materialdried over magnesium sulphate
  7. filtrationfiltered
  8. concentrationconcentrated
  9. customChromatography of the residue on silica gel with toluene and recrystallization from ethanol

출처 및 근거

ORD 기록
ord-d6749063ee40420fa34bbe6a5a7bf53b
출처 데이터셋
uspto-grants-1992_03
특허 번호
US05093027

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