반응식
C(OC(=O)C)(=O)C.C([O-])(=O)C.[K+].[N:13](OCCC(C)C)=O.[C:21]([O:24][C:25]1[CH:30]=[C:29]([CH3:31])[C:28]([NH:32][C:33](=[O:35])[CH3:34])=[CH:27][C:26]=1[CH3:36])(=[O:23])[CH3:22]>[Br-].C([N+](CCCC)(CCCC)CCCC)CCC.C(OCC)(=O)C.O>[C:21]([O:24][C:25]1[CH:30]=[C:29]2[C:28](=[CH:27][C:26]=1[CH3:36])[N:32]([C:33](=[O:35])[CH3:34])[N:13]=[CH:31]2)(=[O:23])[CH3:22]참가 물질
실험 절차
Acetic anhydride (0.96 ml, 10.2 mmol), tetrabutylammonium bromide (55 mg, 0.169 mmol), potassium acetate (665 mg, 6.78 mmol) and isoamyl nitrite (0.592 ml, 4.41 mmol) were added to a solution of 4-(acetylamino)-2,5-dimethylphenyl acetate (750 mg, 3.39 mmol) in ethyl acetate (7.5 ml) at room temperature, and the resulting mixture was refluxed. After 9 hours, the reaction solution was poured into water (50 ml) and extracted with ethyl acetate (50 ml×2), and the organic layer was dried over anhydrous magnesium sulfate. The organic layer dried was concentrated under reduced pressure and the resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate) to obtain 1-acetyl-6-methyl-1H-indazol-5-yl acetate (359 mg, 46%).
후처리
- temperaturethe resulting mixture was refluxed
- extractionextracted with ethyl acetate (50 ml×2)
- dry with materialthe organic layer was dried over anhydrous magnesium sulfate
- customThe organic layer dried
- concentrationwas concentrated under reduced pressure
- customthe resulting residue was purified by a silica gel column chromatography (eluent: hexane/ethyl acetate)
출처 및 근거
- ORD 기록
- ord-3617566acb644d40b8982d67857f84d5
- 출처 데이터셋
- uspto-grants-2007_04
- 특허 번호
- US07199147B2
연결된 노트
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