Salicylaldehyde → HCID 21529337、化合物

HRID 1658386ノート

反応式

HRID 1658386 の反応式
Br[CH2:2][C:3]([C:5]1[CH:6]=[C:7]([CH:11]([CH3:17])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:8]=[CH:9][CH:10]=1)=[O:4].C(=O)([O-])[O-].[K+].[K+].[CH:24]1[CH:29]=[C:28]([CH:30]=O)[C:27]([OH:32])=[CH:26][CH:25]=1>C(O)C>[O:32]1[C:27]2[CH:26]=[CH:25][CH:24]=[CH:29][C:28]=2[CH:30]=[C:2]1[C:3]([C:5]1[CH:6]=[C:7]([CH:11]([CH3:17])[C:12]([O:14][CH2:15][CH3:16])=[O:13])[CH:8]=[CH:9][CH:10]=1)=[O:4]

参加物

5

反応物 3

HCID 6998SalicylaldehydeHCID 11430Potassium CarbonateHCID 21529338HCID 21529338、化合物

生成物 1

HCID 21529337HCID 21529337、化合物収率 25%

試薬・触媒・溶媒 1

HCID 702Ethanol溶媒

実験手順

Ethyl 2-[meta-(α-bromo-acetyl)-phenyl]propionate (0.1 mole) is mixed with dry potassium carbonate (0.2 mole), salicylic aldehyde (0.1 mole) and ethanol (200 cc). The mixture is refluxed for 5 hours, with vigorous stirring. The initially yellow reaction medium turns brown during the heating step. The reaction mixture is then allowed to cool and the resulting precipitate is suction filtered. The alcohol is removed in vacuo. The resulting material is taken up into ethyl acetate, after which it is washed to neutral pH, dried and evaporated. The distilled residue gives a thick oil, b.p.0.05 = 210°-220°C. A second distillation gives the pure product (Yield: 25%).

後処理

  1. temperatureThe mixture is refluxed for 5 hours, with vigorous stirring
  2. temperatureto cool
  3. filtrationfiltered
  4. customThe alcohol is removed in vacuo
  5. washafter which it is washed to neutral pH
  6. customdried
  7. customevaporated
  8. customThe distilled residue gives a thick oil, b.p.0.05 = 210°-220°C
  9. distillationA second distillation

出典と根拠

ORDレコード
ord-bcf48d2e70ce4a20b1933bb4d29115d1
出典データセット
uspto-grants-1976_06
特許番号
US03963758

反応ノート

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