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Water → HCID 15458749, 화합물

HRID 1358540
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HRID 1358540 반응식
[CH:1](=O)[C:2]1[C:3](=[CH:5][CH:6]=[CH:7][CH:8]=1)[OH:4].[CH:10](=[O:18])[CH:11]=[CH:12][CH2:13][CH2:14][CH2:15][CH2:16][CH3:17].C(=O)([O-])[O-].[K+].[K+].O>O1CCOCC1>[CH2:13]([CH:12]1[C:11]([CH:10]=[O:18])=[CH:1][C:2]2[CH:8]=[CH:7][CH:6]=[CH:5][C:3]=2[O:4]1)[CH2:14][CH2:15][CH2:16][CH3:17]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 962WaterHCID 6998SalicylaldehydeHCID 11430Potassium CarbonateHCID 16900Oct-2-enal

생성물 1

HCID 15458749HCID 15458749, 화합물수율 48%

시약·촉매·용매 1

HCID 312751,4-Dioxane용매

실험 절차

A mixture of 22.0 g (0.18 mol) of salicylaldehyde, 25.0 g (0.198 mol) of 2-octenal and 24.8 g (0.18 mol) of potassium carbonate in 200 ml of dioxane, maintained under an inert atmosphere, is heated at reflux for 2.5 h. The reaction mixture is subsequently brought to room temperature (20-25° C.) and then diluted by addition of 1.5 litres of water. The formation of an oil is observed, which oil is extracted with methylene chloride. The organic phase is dried over anhydrous sodium sulphate and then concentrated under reduced pressure. The title compound is thus obtained in a form of an orange oil, which oil is distilled under reduced pressure (B.p. (0.44 mm Hg): 132-140° C.). 20 g of the title product are obtained by distillation (48% yield).

후처리

  1. temperaturemaintained under an inert atmosphere
  2. temperatureis heated
  3. temperatureat reflux for 2.5 h
  4. customis subsequently brought to room temperature
  5. custom(20-25° C.)
  6. extractionwhich oil is extracted with methylene chloride
  7. dry with materialThe organic phase is dried over anhydrous sodium sulphate
  8. concentrationconcentrated under reduced pressure

출처 및 근거

ORD 기록
ord-98a9fa77fd8d43a69c9de7f2d67fc31a
출처 데이터셋
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US06596758B1

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