反应 #64041

反应方程式

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

收率 39.8%

溶剂

ethanol

反应条件

后处理

1. 1
   其他the ethanol was removed by evaporation under reduced pressure
2. 2
   workup.ADDITIONThe residue was treated with dichloromethane
3. 3
   洗涤the organic phase was washed twice with water
4. 4
   干燥dried over anhydrous sodium sulfate
5. 5
   其他The solvent was removed by evaporation under reduced pressure
6. 6
   其他the product recrystallized from ethanol

实验过程

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.

来源