반응식
Cl.[CH2:2]([O:4][NH2:5])[CH3:3].[OH-].[Na+].[OH:8][C:9]1[CH2:14][CH:13]([C:15]2[C:20]([CH3:21])=[C:19]([N+:22]([O-:24])=[O:23])[C:18]([CH3:25])=[C:17]([N+:26]([O-:28])=[O:27])[C:16]=2[CH3:29])[CH2:12][C:11](=[O:30])[C:10]=1[C:31](=O)[CH2:32][CH3:33]>C(O)C>[CH2:2]([O:4][N:5]=[C:31]([C:10]1[C:9](=[O:8])[CH2:14][CH:13]([C:15]2[C:16]([CH3:29])=[C:17]([N+:26]([O-:28])=[O:27])[C:18]([CH3:25])=[C:19]([N+:22]([O-:24])=[O:23])[C:20]=2[CH3:21])[CH2:12][C:11]=1[OH:30])[CH2:32][CH3:33])[CH3:3]참가 물질
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.
후처리
- customthe ethanol was removed by evaporation under reduced pressure
- additionThe residue was treated with dichloromethane
- washthe organic phase was washed twice with water
- dry with materialdried over anhydrous sodium sulfate
- customThe solvent was removed by evaporation under reduced pressure
- customthe product recrystallized from ethanol
출처 및 근거
- ORD 기록
- ord-892533419a0649809487026e6043972a
- 출처 데이터셋
- uspto-grants-1987_05
- 특허 번호
- US04666510
연결된 노트
불러오는 중…