Ethanol → HCID 18317742, 화합물
반응식
ClC1C=CC=CC=1C1C[C:12](=O)[C:11](=[C:15](O)[CH3:16])C(=O)C1.[ClH:19].N(N=[C:25]1[CH2:33][CH:32]([C:34]2[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=2)[CH2:31][C:30]2[NH:29][CH:28]=[C:27]([CH3:40])[C:26]1=2)C(N)=N.[CH2:41]([N:43](CC)CC)[CH3:42].C([OH:50])C>>[CH2:28]([N:29]1[C:30]2[CH2:31][CH:32]([C:34]3[CH:35]=[CH:36][CH:37]=[CH:38][C:39]=3[Cl:19])[CH2:33][C:25](=[O:50])[C:26]=2[C:41]([CH3:42])=[N:43]1)[C:27]1[CH:40]=[CH:12][CH:11]=[CH:15][CH:16]=1참가 물질
5
실험 절차
To a solution of 5-(2-chlorophenyl)-2-(1-hydroxyethylidene)cyclohexane-1,3-dione (0.5 g) and benzylhydrazine 2 hydrochloride (0.39 g) in ethanol (30 ml) was added triethylamine (0.42 g), and the mixture was refluxed for 2.5 hours. Under reduced pressure, the solvent was evaporated, and the residue was dissolved in ethyl acetate. The organic layer was washed with water and saturated brine, dried with magnesium sulfate and concentrated under reduced pressure, and the residue was purified with silica gel column chromatography (ethyl acetate-hexane). The resulting crystals were recrystallized from ethyl acetate-hexane to give 1-benzyl-6-(2-chlorophenyl)-3-methyl-4,5,6,7-tetrahydroindazol-4-one (0.37 g) as colorless crystals.
후처리
- temperaturethe mixture was refluxed for 2.5 hours
- customUnder reduced pressure, the solvent was evaporated
- dissolutionthe residue was dissolved in ethyl acetate
- washThe organic layer was washed with water and saturated brine
- dry with materialdried with magnesium sulfate
- concentrationconcentrated under reduced pressure
- customthe residue was purified with silica gel column chromatography (ethyl acetate-hexane)
- customThe resulting crystals were recrystallized from ethyl acetate-hexane
출처 및 근거
- ORD 기록
- ord-60d4f62dd6514c8eb263f1ed4c0a5848
- 출처 데이터셋
- uspto-grants-2002_02
- 특허 번호
- US06350749B1
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