N-bromobutanimide → 5-(Bromomethyl)-2-chloro-3-fluoropyridine
反応式
[Cl:1][C:2]1[C:7]([F:8])=[CH:6][C:5]([CH3:9])=[CH:4][N:3]=1.[Br:10]N1C(=O)CCC1=O>C(Cl)(Cl)(Cl)Cl.C(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>[Br:10][CH2:9][C:5]1[CH:6]=[C:7]([F:8])[C:2]([Cl:1])=[N:3][CH:4]=1参加物
5
実験手順
4.00 g (27.6 mmol) of 2-chloro-3-fluoro-5-methyl pyridine was dissolved in 80 ml of carbon tetrachloride, 7.37 g (41.4 mmol) of N-bromosuccinimide and 20 mg of benzoyl peroxide were added thereto, and the resulting mixture was heated and refluxed overnight. After the reaction was completed, the reaction solution was returned to room temperature, concentrated under reduced pressure and purified by silica gel column chromatography (hexane:ethyl acetate=19:1) to obtain 3.06 g (yield 51%) of 5-(bromomethyl)-2-chloro-3-fluoropyridine.
後処理
- temperaturethe resulting mixture was heated
- temperaturerefluxed overnight
- customwas returned to room temperature
- concentrationconcentrated under reduced pressure
- custompurified by silica gel column chromatography (hexane:ethyl acetate=19:1)
出典と根拠
- ORDレコード
- ord-0de255f4db904a38a841d8ba9c0a04cb
- 出典データセット
- uspto-grants-2016_04
- 特許番号
- US09301525B2
反応ノート
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