N-bromobutanimide → 3-Bromo-2-methoxy-5-(trifluoromethyl)pyridine
반응식
[CH3:1][O:2][C:3]1[CH:8]=[CH:7][C:6]([C:9]([F:12])([F:11])[F:10])=[CH:5][N:4]=1.C1C(=O)N([Br:20])C(=O)C1>C(#N)C>[Br:20][C:8]1[C:3]([O:2][CH3:1])=[N:4][CH:5]=[C:6]([C:9]([F:12])([F:10])[F:11])[CH:7]=1참가 물질
4
실험 절차
To a stirred solution of 2-methoxy 5-(trifluoromethyl) pyridine (4 g, 22.58 mmol) was dissolved in acetonitrile (50 ml) was added NBS (6 g, 33.87 mmol) portion wise at 0° C. The reaction mixture was stirred for overnight at RT. The solvent was removed under vacuum, quenched with water (100 mL) and extracted with ethyl acetate. The combined organic layer was washed with water, brine, dried over sodium sulfate, and concentrated at reduced pressure to yield 3-bromo-2-methoxy-5-(trifluoromethyl)pyridine (12) as a pale yellow liquid (2 g, 34.7%).
후처리
- customThe solvent was removed under vacuum
- customquenched with water (100 mL)
- extractionextracted with ethyl acetate
- washThe combined organic layer was washed with water, brine
- dry with materialdried over sodium sulfate
- concentrationconcentrated at reduced pressure
출처 및 근거
- ORD 기록
- ord-f8f8aec63b0142a99d32b4aa9a984ed3
- 출처 데이터셋
- uspto-grants-2015_10
- 특허 번호
- US09163020B2
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