Benzoyl Peroxide → 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(OOC(=O)C1C=CC=CC=1)(=O)C1C=CC=CC=1>C(Cl)(Cl)(Cl)Cl>[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
2-chloro-3-fluoro-5-methylpyridine in an amount of 4.00 g (27.6 mmol) was dissolved in 80 mL of carbon tetrachloride, following which 7.37 g (41.4 mmol) of N-bromosuccinimide and 20 mg of benzoyl peroxide were added and the mixture was refluxed overnight under heating. Following reaction completion, the reaction mixture was returned to room temperature, concentrated under reduced pressure, and purified by silica gel column chromatography (hexane/ethyl acetate=19:1), giving 3.06 g of 5-(bromomethyl)-2-chloro-3-fluoropyridine (yield, 51%).
後処理
- additionwere added
- temperaturethe mixture was refluxed overnight
- temperatureunder heating
- customreaction completion
- 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-755bd91c2f3e45649ae7e7b2bcf0baaf
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09328068B2
反応ノート
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