Acetone → HCID 178478397、化合物
反応式
[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]2[NH:8][N:9]=[CH:10][C:3]=12.[I:11]N1C(=O)CCC1=O.CN(C=O)C.CC(C)=O>C(Cl)Cl>[Cl:1][C:2]1[N:7]=[CH:6][N:5]=[C:4]2[NH:8][N:9]=[C:10]([I:11])[C:3]=12参加物
6
反応条件
- 温度
- 50 °C
実験手順
Charge 4-chloro-1H-pyrazolo[3,4-d]pyrimidine (6.1 g, 1.0 eq), N-iodosuccinimide (NIS) (21.55 g, 2.0 eq) and DMF (213.5 mL) in a round bottom flask. Stir the reaction mass at 50° C. for 16 h. Monitor the reaction by TLC (10% acetone in DCM). Concentrate the reaction mass under reduced pressure. Charge ethyl acetate and wash with water and saturated aq. sodium chloride. Dry the organic layer over anhydrous sodium sulfate and concentrate the organic layer under reduced pressure to give 4-chloro-3-iodo-1H-pyrazolo[3,4-d]pyrimidine (6.8 g, 61.43%).
後処理
- concentrationConcentrate the reaction mass under reduced pressure
- washCharge ethyl acetate and wash with water and saturated aq. sodium chloride
- dry with materialDry the organic layer over anhydrous sodium sulfate
- concentrationconcentrate the organic layer under reduced pressure
出典と根拠
- ORDレコード
- ord-f2e27979dc644150a5f36d212d67cea4
- 出典データセット
- uspto-grants-2012_01
- 特許番号
- US08093383B2
反応ノート
読み込み中…