N-bromobutanimide → HCID 86646794, 화합물
반응식
[CH3:1][N:2]1[C:6]([CH3:7])=[C:5]([C:8](=[O:10])C)[CH:4]=[N:3]1.[Br:11]N1C(=O)CCC1=O>C1COCC1.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:11][CH2:7][C:6]1[N:2]([CH3:1])[N:3]=[CH:4][C:5]=1[CH:8]=[O:10]참가 물질
5
실험 절차
To a stirred solution of 1-(1,5-dimethyl-1H-pyrazol-4-yl)ethanone (471 mg, 3.42 mmol) in THF (13 ml) was added N-bromosuccinimide (637 mg, 3.58 mmol) and benzoyl peroxide (41 mg, 0.17 mmol) at room temperature under nitrogen, then the resulting mixture was refluxed for 20 h. After cooling, the reaction mixture was evaporated to remove the solvents. The residue was chromatographed on a column of silica gel eluting with ethyl acetate-hexane (1:1) gave the title compound as white solid (574 mg, 78% yield). 1H NMR (270 MHz, CDCl3) 2.47 (3H, s), 3.91 (3H, s), 4.87 (2H, s), 7.83 (1H, s). MS (ESI) m/z: 217 (M+H)+.
후처리
- temperaturethe resulting mixture was refluxed for 20 h
- temperatureAfter cooling
- customthe reaction mixture was evaporated
- customto remove the solvents
- customThe residue was chromatographed on a column of silica gel eluting with ethyl acetate-hexane (1:1)
출처 및 근거
- ORD 기록
- ord-979b3ff1591c4a0f9986c7a856d38313
- 출처 데이터셋
- uspto-grants-2011_06
- 특허 번호
- US07964732B2
반응 노트
불러오는 중…