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

HRID 1901357노트

반응식

HRID 1901357 반응식
[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

참가 물질

5

반응물 3

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

생성물 1

HCID 218443705-Bromo-2-(4-methoxybenzyl)benzofuran수율 82.5%

시약·촉매·용매 1

HCID 8117Diethylene Glycol용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-d829c7ee9fbc42eab859867b19cfd640
출처 데이터셋
uspto-grants-1996_11
특허 번호
US05576343

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