Ethanol → 8-Hydroxyjulolidine

HRID 2303940

反応式

HRID 2303940 の反応式
[NH2:1][C:2]1[CH:3]=[C:4]([OH:8])[CH:5]=[CH:6][CH:7]=1.Br[CH2:10][CH2:11][CH2:12]Cl.[C:14]([O-])(O)=O.[Na+].[CH2:19](O)[CH3:20]>>[CH2:11]1[CH2:12][N:1]2[C:2]3[C:3]([CH2:14][CH2:19][CH2:20]2)=[C:4]([OH:8])[CH:5]=[CH:6][C:7]=3[CH2:10]1

参加物

5

反応物 4

HCID 702EthanolHCID 80061-Bromo-3-chloropropaneHCID 115683-AminophenolHCID 516892Sodium Bicarbonate

生成物 1

HCID 1704748-Hydroxyjulolidine収率 35%

実験手順

m-Aminophenol (1.1 g, 10 mmol), 1-bromo-3-chloropropane (4.8 g, 3 ml, 30 mmol) and ethanol (10 ml) were placed in a 100 ml two-necked round-bottomed flask. The mixture was heated and refluxed for 11 hours, during which an NaHCO3 aqueous solution (2.0 g, 20 ml, 23 mmol) was added. The mixture was further heated and refluxed for 37 hours. The solvent was removed by distillation under reduced pressure. The resulting crude product was extracted with hexane by a solid-liquid continuous extraction to give 8-hydroxyjulolidine (661 mg) in 35% yield.

後処理

  1. temperatureThe mixture was heated
  2. additionwas added
  3. temperatureThe mixture was further heated
  4. temperaturerefluxed for 37 hours
  5. customThe solvent was removed by distillation under reduced pressure
  6. extractionThe resulting crude product was extracted with hexane by a solid-liquid continuous extraction

出典と根拠

ORDレコード
ord-e3674b5e94114bc79142154a9fbf5eb4
出典データセット
uspto-grants-2002_08
特許番号
US06433176B1

関連ノート

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