Hydrochloric Acid → 5-Bromo-3-morpholinopyridin-2-ol
반응식
[Br:1][C:2]1[CH:3]=[C:4]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[C:5]([O:8]C)=[N:6][CH:7]=1.Cl>O1CCOCC1>[Br:1][C:2]1[CH:3]=[C:4]([N:10]2[CH2:15][CH2:14][O:13][CH2:12][CH2:11]2)[C:5](=[O:8])[NH:6][CH:7]=1참가 물질
4
반응 조건
- 온도
- 100 °C
실험 절차
To a solution of 4-(5-bromo-2-methoxypyridin-3-yl)morpholine (1.0 equiv.) in 1,4-dioxane (0.3 M) was added concentrated HCl (5 equiv.) and the solution was heated to 100° C. for 1 h. Upon cooling to room temperature, the solution was concentrated to dryness under vacuo, then dissolved in water and neutralized with solid sodium bicarbonate. The precipitate was filtered, washed with water and dried under vacuo to give 5-bromo-3-morpholinopyridin-2(1H)-one as a beige solid in 93% yield. LCMS m/z (M+H)=258.9/260.9, Rt=0.48 min.
후처리
- temperatureUpon cooling to room temperature
- concentrationthe solution was concentrated to dryness under vacuo
- dissolutiondissolved in water and neutralized with solid sodium bicarbonate
- filtrationThe precipitate was filtered
- washwashed with water
- customdried under vacuo
출처 및 근거
- ORD 기록
- ord-c7c0573354f94c41b214776f9f52d15f
- 출처 데이터셋
- uspto-grants-2016_01
- 특허 번호
- US09242969B2
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