N-bromobutanimide → 5-(Bromomethyl)-2-chloro-3-fluoropyridine
반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-0de255f4db904a38a841d8ba9c0a04cb
- 출처 데이터셋
- uspto-grants-2016_04
- 특허 번호
- US09301525B2
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