N-bromobutanimide → 5-Bromo-2-(1-bromoethyl)pyridine
反応式
[CH2:1]([C:3]1[CH:8]=[CH:7][C:6]([Br:9])=[CH:5][N:4]=1)[CH3:2].[Br:10]N1C(=O)CCC1=O>ClCCCl>[Br:10][CH:1]([C:3]1[CH:8]=[CH:7][C:6]([Br:9])=[CH:5][N:4]=1)[CH3:2]参加物
4
実験手順
A solution of 2-ethyl-5-bromopyridine (1.86 g, 10 mmol), N-bromosuccinimide (1.78 g, 10 mmol) in 1,2-dichloroethane (20 ml) was brought to reflux before the addition of azoisobutyronitrile (AIBN) (20 mg). The solution was then refluxed for a further two hours. The cooled suspension was filtered and evaporated in vacuo. Purification by column chromatography (silica gel, eluting with 1:1 dichloromethane/hexane) gave the desired product as a pale yellow oil (2.12 g, 80%).
後処理
- temperatureThe solution was then refluxed for a further two hours
- filtrationThe cooled suspension was filtered
- customevaporated in vacuo
- customPurification
- washby column chromatography (silica gel, eluting with 1:1 dichloromethane/hexane)
出典と根拠
- ORDレコード
- ord-a273fbe0a5ce4e9ba3d01fa0568a7cf2
- 出典データセット
- uspto-grants-2000_01
- 特許番号
- US06015825
反応ノート
読み込み中…