반응 #82268

반응 방정식

potassium hydroxide

hydrazine dihydrate

5-bromo-2-(4-methoxybenzoyl)benzofuran

→

5-bromo-2-(4-methoxybenzyl)benzofuran

수율 82.5%

용매

diethylene glycol

반응 조건

후처리

1. 1
   온도The thus prepared mixture was refluxed
2. 2
   온도under heating
3. 3
   온도After cooling
4. 4
   기타the resulting reaction solution
5. 5
   추출extracted with benzene
6. 6
   기타dried
7. 7
   workup.DISTILLATIONAfter distilling off the solvent
8. 8
   기타the resulting residue was purified

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.

출처