N-bromobutanimide → 3-Bromo-2-(bromomethyl)benzonitrile
反応式
C1C(=O)N([Br:8])C(=O)C1.[Br:9][C:10]1[C:11]([CH3:18])=[C:12]([CH:15]=[CH:16][CH:17]=1)[C:13]#[N:14]>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:9][C:10]1[C:11]([CH2:18][Br:8])=[C:12]([CH:15]=[CH:16][CH:17]=1)[C:13]#[N:14]参加物
5
実験手順
A mixture of NBS (3.45 g), dibenzoyl peroxide (100 mg) and 3-bromo-2-methylbenzonitrile (3.47 g) in carbon tetrachloride (40 ml) was heated at reflux under nitrogen for 48 h. The mixture was then cooled to room temperature, filtered and concentrated in vacuo to give a pale yellow solid. Chromatography eluting with dichloromethane gave the title compound as a white solid (4.23 g) m.p. 90°-93° C.
後処理
- temperaturewas heated
- temperatureat reflux under nitrogen for 48 h
- filtrationfiltered
- concentrationconcentrated in vacuo
- customto give a pale yellow solid
- washChromatography eluting with dichloromethane
出典と根拠
- ORDレコード
- ord-0dcdab110f0f46959854301c623b7893
- 出典データセット
- uspto-grants-1994_12
- 特許番号
- US05374646
反応ノート
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