Acetone → HCID 178478397, 화합물
반응식
[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]=12참가 물질
6
반응 조건
- 온도
- 50 °C
실험 절차
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%).
후처리
- 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
출처 및 근거
- ORD 기록
- ord-f2e27979dc644150a5f36d212d67cea4
- 출처 데이터셋
- uspto-grants-2012_01
- 특허 번호
- US08093383B2
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