반응 #64041

반응 방정식

Ethoxyaminehydrochloride

sodium hydroxide

3-hydroxy-5-(2,4,6-trimethyl-3,5-dinitrophenyl)-2-propionylcyclohex-2-en-1-one

→

2-[1-(ethoxyimino)propyl]-3-hydroxy-5-(2,4,6-trimethyl-3,5-dinitrophenyl)cyclohex-2-en-1-one

수율 39.8%

용매

ethanol

반응 조건

후처리

1. 1
   기타the ethanol was removed by evaporation under reduced pressure
2. 2
   workup.ADDITIONThe residue was treated with dichloromethane
3. 3
   세척the organic phase was washed twice with water
4. 4
   건조dried over anhydrous sodium sulfate
5. 5
   기타The solvent was removed by evaporation under reduced pressure
6. 6
   기타the product recrystallized from ethanol

실험 절차

Ethoxyaminehydrochloride (0.36 g, 3.7 mmole) and then sodium hydroxide (0.15 g, 3.7 mmole) were added to a solution of 3-hydroxy-5-(2,4,6-trimethyl-3,5-dinitrophenyl)-2-propionylcyclohex-2-en-1-one (1.0 g; 2.7 mmole) in absolute ethanol (80 ml). The mixture was stirred at room temperature for a period of 24 hours and then the ethanol was removed by evaporation under reduced pressure. The residue was treated with dichloromethane and the organic phase was washed twice with water and then dried over anhydrous sodium sulfate. The solvent was removed by evaporation under reduced pressure and the product recrystallized from ethanol to give 2-[1-(ethoxyimino)propyl]-3-hydroxy-5-(2,4,6-trimethyl-3,5-dinitrophenyl)cyclohex-2-en-1-one (0.45 g; 39.8%) as a white solid, mp 170° C.

출처