반응 #5097

반응 방정식

2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one

hydroxylamine hydrochloride

pyridine

→

2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one oxime

용매

ethyl acetate

ethanol

ethanol

반응 조건

후처리

1. 1
   온도was refluxed for 4 hours
2. 2
   농축the reaction mixture was concentrated to dryness under a reduced pressure
3. 3
   기타the residue thus obtained
4. 4
   세척washed three times with 1 liter of water each time
5. 5
   기타the residue was dried again under a reduced pressure
6. 6
   기타Recrystallized from ethyl acetate/n-hexane mixture

실험 절차

An ethanol solution containing 120 g of 2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one, 45 of hydroxylamine hydrochloride and 200 ml of pyridine in 1,200 ml of ethanol was refluxed for 4 hours. After the reaction was completed, the reaction mixture was concentrated to dryness under a reduced pressure, then the residue thus obtained was dissolved in 2 liters of ethyl acetate and washed three times with 1 liter of water each time, and the residue was dried again under a reduced pressure. Recrystallized from ethyl acetate/n-hexane mixture to obtain 90 g of 2,3-dihydro-7-hydroxy-4-methyl-6-(1-phenyl-2-propenyl)-1H-inden-1-one oxime. Light yellow flake-like crystals. Melting point: 146° C. (Decomposed).

출처