반응 #5093

반응 방정식

2,3-dihydro-4,6-dimethyl-7-hydroxy-2-(4-methoxybenzylidene)-1H-inden-1-one

hydrogen

→

2,3-dihydro-4, 6-dimethyl-7-hydroxy-2-(4-methoxybenzyl)-1H-inden-1-one

용매

ethylacetate

acetic acid

반응 조건

후처리

1. 1
   기타After the catalytic reduction, the catalyst was removed by filtration
2. 2
   농축the filtrate was concentrated
3. 3
   기타by removing the solvent under reduced pressure
4. 4
   기타The residue thus obtained
5. 5
   기타was purified by a silica gel column chromatography (eluent: n-hexane: ethyl acetate=9:1)

실험 절차

16.09 Grams of 2,3-dihydro-4,6-dimethyl-7-hydroxy-2-(4-methoxybenzylidene)-1H-inden-1-one was dissolved in a mixed solvent of 150 ml of ethylacetate with 100 ml of acetic acid, this solution was let subjected to catalytic reduction at room temperature under 3 atmospheric hydrogen gas pressure in the presence of 1.5 g of palladium black as the hydrogenation catalyst. After the catalytic reduction, the catalyst was removed by filtration, and the filtrate was concentrated by removing the solvent under reduced pressure. The residue thus obtained was purified by a silica gel column chromatography (eluent: n-hexane: ethyl acetate=9:1) to obtain 8.5 g of 2,3-dihydro-4, 6-dimethyl-7-hydroxy-2-(4-methoxybenzyl)-1H-inden-1-one as in the form of colorless oily substance.

출처