Methyl iodide → (6-Bromo-5-methoxypyridin-2-yl)methanol
반응식
[Br:1][C:2]1[C:7]([OH:8])=[CH:6][CH:5]=[C:4]([CH2:9][OH:10])[N:3]=1.[C:11]([O-])([O-])=O.[K+].[K+].IC>CC(C)=O>[Br:1][C:2]1[N:3]=[C:4]([CH2:9][OH:10])[CH:5]=[CH:6][C:7]=1[O:8][CH3:11]참가 물질
5
실험 절차
To a solution of 2-bromo-6-(hydroxymethyl)pyridin-3-ol (2.04 g, 10 mmol) and K2CO3 (2.07 g, 15 mmol) in acetone (50 mL) was added iodomethane (1.84 g, 13 mmol) at rt. The reaction mixture was refluxed for 4 h. After that time the reaction was cooled to rt, filtered to remove solids and concentrated under reduced pressure to give (6-bromo-5-methoxypyridin-2-yl)methanol (3.42 g, >99%) as a white solid: 1H NMR (400 MHz, CDCl3): δ 7.25 (d, J=8.0 Hz, 1H), 7.16 (d, J=8.4 Hz, 1H), 4.70 (s, 2H), 3.93 (s, 3H), 2.78 (br s, 1H).
후처리
- temperatureThe reaction mixture was refluxed for 4 h
- filtrationfiltered
- customto remove solids
- concentrationconcentrated under reduced pressure
출처 및 근거
- ORD 기록
- ord-55bb34e9e2954b129a7f2d432c0df325
- 출처 데이터셋
- uspto-grants-2015_07
- 특허 번호
- US09073878B2
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