2,4-Dichloro-5-fluoropyrimidine → HCID 57562949、化合物
反応式
[F:1][CH2:2][CH2:3][CH2:4][C:5]1[CH:11]=[CH:10][C:8]([NH2:9])=[CH:7][CH:6]=1.[Cl:12][C:13]1[N:18]=[CH:17][C:16]([F:19])=[C:15](Cl)[N:14]=1>CO.O>[Cl:12][C:13]1[N:18]=[C:17]([NH:9][C:8]2[CH:10]=[CH:11][C:5]([CH2:4][CH2:3][CH2:2][F:1])=[CH:6][CH:7]=2)[C:16]([F:19])=[CH:15][N:14]=1参加物
5
実験手順
4-(3-Fluoropropyl)aniline and 2,6-dichloro-5-fluoropyrimidine (1.5 g) were dissolved in methanol (5 mL) and water (1 mL). The reaction solution was stirred at rt for 3 d. The reaction solution was diluted with water (100 mL) and extracted with ethyl acetate (2×100 mL). The organic layers were evaporated and purified by flash column chromatography (EtOAc/hexanes=1/4, 1/2) to give 2-chloro-5-fluoro-N4-[4-(3-fluoropropyl)phenyl]-4-pyrimidineamine.
後処理
- extractionextracted with ethyl acetate (2×100 mL)
- customThe organic layers were evaporated
- custompurified by flash column chromatography (EtOAc/hexanes=1/4, 1/2)
出典と根拠
- ORDレコード
- ord-e5ad2cabdef54e089dd9b50b4474ddcc
- 出典データセット
- uspto-grants-2013_04
- 特許番号
- US08415365B2
反応ノート
読み込み中…