Benzoyl Peroxide → Methyl 4-(bromomethyl)-6-chloronicotinate
반응식
[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]=1참가 물질
5
실험 절차
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.
후처리
- 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%)
출처 및 근거
- ORD 기록
- ord-75aeff83ff1645f8a7edc269fd1c37b4
- 출처 데이터셋
- uspto-grants-2014_11
- 특허 번호
- US08895571B2
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