N-Iodosuccinimide → 6-Chloro-5-iodopyrimidin-4-amine
反応式
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH2:8])[CH:3]=1.[I:9]N1C(=O)CCC1=O>CN(C)C=O.O.C(OCC)(=O)C>[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[I:9]参加物
6
実験手順
To a solution of 6-chloropyrimidin-4-amine (1 g, 7.8 mmol) in 5 mL N,N-dimethylformamide was added N-iodosuccinimide (2.6 g, 11.6 mmol) and the mixture subjected to microwave irradiation (Biotage Initiator) at 100° C. for 30 minutes. The mixture was diluted with water and ethyl acetate and the ethyl acetate layer was washed with water and brine, dried over sodium sulfate, filtered, and concentrated. Purification by column chromatography (silica gel, 25% ethyl acetate in hexane) afforded the title compound. LCMS: 255.91 (M+1)+.
後処理
- customthe mixture subjected to microwave irradiation (Biotage Initiator) at 100° C. for 30 minutes
- washthe ethyl acetate layer was washed with water and brine
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customPurification by column chromatography (silica gel, 25% ethyl acetate in hexane)
出典と根拠
- ORDレコード
- ord-b694db7943114eb19921b039e6774af2
- 出典データセット
- uspto-grants-2016_05
- 特許番号
- US09346813B2
反応ノート
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