Bromine → 4-Bromo-7-methoxy-1-benzofuran-2-carbaldehyde

HRID 1108316ノート

反応式

HRID 1108316 の反応式
[CH:1]([C:3]1[O:4][C:5]2[C:11]([O:12][CH3:13])=[CH:10][CH:9]=[CH:8][C:6]=2[CH:7]=1)=[O:2].C([O-])(=O)C.[Na+].[Br:19]Br>ClCCl>[CH:1]([C:3]1[O:4][C:5]2[C:11]([O:12][CH3:13])=[CH:10][CH:9]=[C:8]([Br:19])[C:6]=2[CH:7]=1)=[O:2]

参加物

5

反応物 3

HCID 24408BromineHCID 517045Sodium AcetateHCID 34573107-Methoxy-1-benzofuran-2-carbaldehyde

生成物 1

HCID 187848644-Bromo-7-methoxy-1-benzofuran-2-carbaldehyde

試薬・触媒・溶媒 1

HCID 6344Dichloromethane溶媒3 回

実験手順

2-Formyl-7-methoxybenzofuran (1.0 g) was stirred in dichloromethane (10 ml) under nitrogen at 0° C. Sodium acetate (1.4 g) was added followed by the dropwise addition of bromine (0.29 ml). Further dichloromethane (20 ml) was added to the mixture to facilitate stirring and the mixture was stirred overnight. The reaction mixture was diluted with dichloromethane (40 ml) and washed with water (30 ml). Drying over magnesium sulfate followed by removal of the solvent in vacuo gave a pale orange solid. Purification by flash chromatography on silica eluting with 10% ethyl acetate in hexane gave the title compound (0.50 g) as a beige solid.

後処理

  1. stirringthe mixture was stirred overnight
  2. washwashed with water (30 ml)
  3. dry with materialDrying over magnesium sulfate
  4. customfollowed by removal of the solvent in vacuo
  5. customgave a pale orange solid
  6. customPurification by flash chromatography on silica eluting with 10% ethyl acetate in hexane

出典と根拠

ORDレコード
ord-7eb9a6b965734d07987a37983b422353
出典データセット
uspto-grants-2000_05
特許番号
US06066657

反応ノート

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