N-bromobutanimide → 5-Bromo-3-(trifluoromethyl)pyridin-2-amine
반응식
[F:1][C:2]([F:11])([F:10])[C:3]1[C:4]([NH2:9])=[N:5][CH:6]=[CH:7][CH:8]=1.[Br:12]N1C(=O)CCC1=O>CC#N>[Br:12][C:7]1[CH:8]=[C:3]([C:2]([F:1])([F:10])[F:11])[C:4]([NH2:9])=[N:5][CH:6]=1참가 물질
4
실험 절차
To a solution of 3-trifluoromethyl-pyridin-2-ylamine (Fluorochem Ltd., Derbyshire, United Kingdom, 5.37 g, 32.8 mmol) in 100 ml of dry CH3CN under argon were added N-bromosuccinimide (6.45 g, 36.2 mmol) in 4 equal portions over a period of 1 h at 0-5° C. The cooling bath was removed and stirring was continued for 3 h. The solvent was evaporated under vacuum, then the residue was dissolved in EtOAc and washed with water and brine. The organic layer was dried over Na2SO4 and evaporated to give the title compound as a orange oil. (M+H=239; 241).
후처리
- customThe cooling bath was removed
- customThe solvent was evaporated under vacuum
- dissolutionthe residue was dissolved in EtOAc
- washwashed with water and brine
- dry with materialThe organic layer was dried over Na2SO4
- customevaporated
출처 및 근거
- ORD 기록
- ord-f6d7c9ae79934660842df9765f08cf0f
- 출처 데이터셋
- uspto-grants-2013_07
- 특허 번호
- US08476294B2
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