1,2-Dibromoethane → 8-Fluoro-2,3-dihydro-1,4-benzodioxin-6-carboxaldehyde

HRID 15308

反応式

HRID 15308 の反応式
[F:1][C:2]1[CH:3]=[C:4]([CH:7]=[C:8]([OH:11])[C:9]=1[OH:10])[CH:5]=[O:6].C(=O)([O-])[O-].[K+].[K+].Br[CH2:19][CH2:20]Br>CN(C=O)C>[F:1][C:2]1[C:9]2[O:10][CH2:19][CH2:20][O:11][C:8]=2[CH:7]=[C:4]([CH:5]=[O:6])[CH:3]=1

参加物

5

実験手順

To a solution of 3-fluoro-4,5-dihydroxybenzaldehyde (0.66 g, 4.2 mmol) in DMF (30 ml) was added potassium carbonate (1.15 g, 8.3 mmol) and 1,2-dibromoethane (0.72 ml, 8.3 mmol) and the resultant mixture was heated to 80° C. for 18 h before the solvent was removed under reduced pressure. The reaction mixture was then treated with dichloromethane and water. The aqueous phase was extracted twice with dichloromethane and the combined organic phases were dried and the solvent was removed under reduced pressure to give the desired compound as a cream solid (0.73 g, 95%).

後処理

  1. customwas removed under reduced pressure
  2. additionThe reaction mixture was then treated with dichloromethane and water
  3. extractionThe aqueous phase was extracted twice with dichloromethane
  4. customthe combined organic phases were dried
  5. customthe solvent was removed under reduced pressure

出典と根拠

ORDレコード
ord-ae2de73b0a5c4c679f9b21e0b468d267
出典データセット
uspto-grants-2010_06
特許番号
US07732461B2

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