Methanol → 2-chloro-5-fluoro-N-methylpyrimidin-4-amine
반응식
[F:1][C:2]1[C:3](Cl)=[N:4][C:5]([Cl:8])=[N:6][CH:7]=1.CO.[CH3:12][NH2:13].CCOC(C)=O>C(O)C.CCCCCCC>[Cl:8][C:5]1[N:4]=[C:3]([NH:13][CH3:12])[C:2]([F:1])=[CH:7][N:6]=1참가 물질
7
실험 절차
To a 250 mL round bottom flask equipped with a stir bar was added 9.0 g 5-fluoro-2,4-dichloro-pyrimidine, 40 mL methanol and 15 mL of 8M methylamine in ethanol. The reaction heated up (mild exo-therm) and was allowed to stir at room temperature for ˜30 minutes. A check by TLC (1:1 EtOAc: heptane) and LCMS showed complete reaction. The reaction was concentrated down to give 9.77 g crude material which was purified on a silica column running a gradient of 1% to 10% MeOH in DCM over 35 minutes to give 6.77 g pure 2-chloro-5-fluoro-N-methylpyrimidin-4-amine
후처리
- customTo a 250 mL round bottom flask equipped with a stir bar
- temperatureThe reaction heated up (mild exo-therm)
- customreaction
- concentrationThe reaction was concentrated down
- customto give 9.77 g crude material which
- customwas purified on a silica column
- customover 35 minutes
출처 및 근거
- ORD 기록
- ord-0c07390f411c4aa5809f1ca454fa1c98
- 출처 데이터셋
- uspto-grants-2013_01
- 특허 번호
- US08354420B2
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