N-bromobutanimide → HCID 86646794、化合物
反応式
[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]参加物
5
実験手順
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)+.
後処理
- 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)
出典と根拠
- ORDレコード
- ord-979b3ff1591c4a0f9986c7a856d38313
- 出典データセット
- uspto-grants-2011_06
- 特許番号
- US07964732B2
反応ノート
読み込み中…