Methanol → 2-chloro-5-fluoro-N-methylpyrimidin-4-amine
反応式
[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]=1参加物
7
実験手順
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.
後処理
- 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
出典と根拠
- ORDレコード
- ord-7fce18595907402187dafbeaffcceae0
- 出典データセット
- uspto-grants-2014_08
- 特許番号
- US08796296B2
反応ノート
読み込み中…