N-Iodosuccinimide → 7-Bromo-3-chloro-8-iodoisoquinoline
反応式
[Br:1][C:2]1[CH:11]=[C:10]2[C:5]([CH:6]=[C:7]([Cl:12])[N:8]=[CH:9]2)=[CH:4][CH:3]=1.C1C(=O)N([I:20])C(=O)C1>S(O)(C(F)(F)F)(=O)=O>[Br:1][C:2]1[C:11]([I:20])=[C:10]2[C:5]([CH:6]=[C:7]([Cl:12])[N:8]=[CH:9]2)=[CH:4][CH:3]=1参加物
4
実験手順
To a flask containing 7-Bromo-3-chloroisoquinoline (1.5 g, 6.19 mmol) was added NIS (1.4 g, 6.9 mmol). The flask was placed in an ice bath and treated with TfOH (40 mL) and stirred at RT overnight. The reaction mixture was carefully poured into ice, and the aqueous layer was extracted with DCM. The combined extracts were washed with brine, dried over Na2SO4, and concentrated under reduced pressure. The crude residue was purified by silica gel column chromatography (Hexanes:DCM→1:1) to provide the title product.
後処理
- customThe flask was placed in an ice bath
- additionThe reaction mixture was carefully poured into ice
- extractionthe aqueous layer was extracted with DCM
- washThe combined extracts were washed with brine
- dry with materialdried over Na2SO4
- concentrationconcentrated under reduced pressure
- customThe crude residue was purified by silica gel column chromatography (Hexanes:DCM→1:1)
出典と根拠
- ORDレコード
- ord-ed496408991d4f62b8fd0a4513bf584d
- 出典データセット
- uspto-grants-2015_04
- 特許番号
- US08999991B2
反応ノート
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