Benzoyl Peroxide → Methyl 4-(bromomethyl)-6-chloronicotinate
反応式
[Cl:1][C:2]1[CH:11]=[C:10]([CH3:12])[C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][N:3]=1.[Br:13]N1C(=O)CCC1=O.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[Br:13][CH2:12][C:10]1[C:5]([C:6]([O:8][CH3:9])=[O:7])=[CH:4][N:3]=[C:2]([Cl:1])[CH:11]=1参加物
5
実験手順
A mixture of methyl 6-chloro-4-methylnicotinate (2.50 g, 13.5 mmol), N-bromosuccinimide (2.88 g, 16.2 mmol) and benzoyl peroxide (0.14 g, 0.56 mmol) in carbon tetrachloride (100 mL) was refluxed under an atmosphere of nitrogen overnight. The mixture was cooled to room temperature, and filtered through a pad of celite. The mixture was concentrated. The residue was purified by combi-flash chromatography (ethyl acetate in hexanes: 30%) to afford the desired product.
後処理
- temperaturewas refluxed under an atmosphere of nitrogen overnight
- filtrationfiltered through a pad of celite
- concentrationThe mixture was concentrated
- customThe residue was purified by combi-flash chromatography (ethyl acetate in hexanes: 30%)
出典と根拠
- ORDレコード
- ord-75aeff83ff1645f8a7edc269fd1c37b4
- 出典データセット
- uspto-grants-2014_11
- 特許番号
- US08895571B2
反応ノート
読み込み中…