Iodine chloride → 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]Cl>CN(C)C=O>[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]([NH2:8])[C:3]=1[I:9]参加物
4
反応条件
- 温度
- 45 °C
実験手順
To a solution of 3.03 g (23.39 mmol) of 6-chloropyrimidin-4-amine in 60 mL of dimethylformamide was added dropwise a solution of iodine monochloride (2.34 mL, 46.70 mmol) in 40 mL of dimethylformamide. Then the mixture was stirred at 45° C. overnight. The solvent was evaporated under reduced pressure and the residue was partitioned between dichloromethane and a 4% aqueous solution of sodium bicarbonate. The organic layer was washed with water and brine, dried over magnesium sulphate, filtered and the solvent was removed in vacuum. The product was purified by flash chromatography (0% to 20%, methanol-dichloromethane) to obtain 4.28 g (72% yield) of the title compound.
後処理
- customThe solvent was evaporated under reduced pressure
- customthe residue was partitioned between dichloromethane
- washThe organic layer was washed with water and brine
- dry with materialdried over magnesium sulphate
- filtrationfiltered
- customthe solvent was removed in vacuum
- customThe product was purified by flash chromatography (0% to 20%, methanol-dichloromethane)
出典と根拠
- ORDレコード
- ord-8ee1ac66138d4b39a5f3ea2a31b43c64
- 出典データセット
- uspto-grants-2016_07
- 特許番号
- US09388189B2
反応ノート
読み込み中…