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Acetic Acid → HCID 367965、化合物

HRID 2286529
ノート
印刷プレビュー

反応式

HRID 2286529 の反応式
[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=O)=[CH:4][CH:3]=1.[OH-].[K+].[CH:12](=[O:15])[CH2:13][CH3:14].C(O)(=O)C>C(O)C>[F:1][C:2]1[CH:9]=[CH:8][C:5]([CH:6]=[C:13]([CH3:14])[CH:12]=[O:15])=[CH:4][CH:3]=1
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 176Acetic AcidHCID 527PropanalHCID 14797Potassium HydroxideHCID 680234-Fluorobenzaldehyde

生成物 1

HCID 367965HCID 367965、化合物収率 77%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒2 回

実験手順

To a solution of 124 g (1 mole) of 4-fluorobenzaldehyde and 8 g (0.143 mole) of potassium hydroxide in 500 ml ethanol at room temperature was added dropwise a solution of 52.2 g (0.9 mole) of propionaldehyde in 100 ml ethanol. After stirring for 0.5 hour, the mixture was acidified with acetic acid and concentrated by rotary evaporation. The residue was partitioned between methylene chloride and water. The aqueous layer was extracted three times with additional methylene chloride. The combined organic layers were dried and concentrated. Distillation through a 12-inch vacuum jacketed column gave 113.5 g (77%) of pale yellow low-melting crystalline product, b.p. 70°-72° C. (0.4-0.7 mm).

後処理

  1. concentrationconcentrated by rotary evaporation
  2. customThe residue was partitioned between methylene chloride and water
  3. extractionThe aqueous layer was extracted three times with additional methylene chloride
  4. customThe combined organic layers were dried
  5. concentrationconcentrated
  6. distillationDistillation through a 12-inch vacuum

出典と根拠

ORDレコード
ord-1660676866b94bc5acc71efe6f3d27ac
出典データセット
uspto-grants-1981_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US04267190

反応ノート

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