Potassium Hydroxide → 5-Bromo-2-(4-methoxybenzyl)benzofuran

HRID 53990

反応式

HRID 53990 の反応式
[OH-].[K+].O.O.NN.[Br:7][C:8]1[CH:9]=[CH:10][C:11]2[O:15][C:14]([C:16](=O)[C:17]3[CH:22]=[CH:21][C:20]([O:23][CH3:24])=[CH:19][CH:18]=3)=[CH:13][C:12]=2[CH:26]=1>C(O)COCCO>[Br:7][C:8]1[CH:9]=[CH:10][C:11]2[O:15][C:14]([CH2:16][C:17]3[CH:18]=[CH:19][C:20]([O:23][CH3:24])=[CH:21][CH:22]=3)=[CH:13][C:12]=2[CH:26]=1

参加物

5

反応物 3

HCID 14797Potassium HydroxideHCID 23717245-Bromo-2-(4-methoxybenzoyl)benzofuranHCID 22141362Hydrazine--water (1/2)

生成物 1

HCID 218443705-Bromo-2-(4-methoxybenzyl)benzofuran収率 82.5%

試薬・触媒・溶媒 1

HCID 8117Diethylene Glycol溶媒

実験手順

5.07 g of potassium hydroxide was added to 30 ml of diethylene glycol, and the mixture was stirred at room temperature during which 5.5 g of 80% hydrazine dihydrate.2H2O and 5.0 g of 5-bromo-2-(4-methoxybenzoyl)benzofuran were further added. The thus prepared mixture was refluxed under heating. After cooling, the resulting reaction solution was adjusted to pH 4-5, extracted with benzene, and then dried. After distilling off the solvent, the resulting residue was purified by subjecting it to silica gel column chromatography using a n-hexane/isopropanol mixture as an elution solvent, thereby obtaining 3.95 g of 5-bromo-2-(4-methoxybenzyl)benzofuran as a brown oily material.

後処理

  1. temperatureThe thus prepared mixture was refluxed
  2. temperatureunder heating
  3. temperatureAfter cooling
  4. customthe resulting reaction solution
  5. extractionextracted with benzene
  6. customdried
  7. distillationAfter distilling off the solvent
  8. customthe resulting residue was purified

出典と根拠

ORDレコード
ord-7b048a536902418b8f4734ceb90042f5
出典データセット
uspto-grants-1997_04
特許番号
US05620991

関連ノート

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