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Water → HCID 15458749、化合物

HRID 1358540
ノート
印刷プレビュー

反応式

HRID 1358540 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

HCID 15458749HCID 15458749、化合物収率 48%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-98a9fa77fd8d43a69c9de7f2d67fc31a
出典データセット
uspto-grants-2003_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06596758B1

反応ノート

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