N-Iodosuccinimide → 7-Bromo-5-iodo-1,2,3-benzothiadiazol-4-amine
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([NH2:11])=[C:6]2[C:10]=1[S:9][N:8]=[N:7]2.C1C(=O)N([I:19])C(=O)C1>C1COCC1>[Br:1][C:2]1[CH:3]=[C:4]([I:19])[C:5]([NH2:11])=[C:6]2[C:10]=1[S:9][N:8]=[N:7]2参加物
4
実験手順
A mixture of 7-bromo-1,2,3-benzothiadiazol-4-amine (80.0 mg, 0.348 mmol) and NIS (117.3 mg, 0.522 mmol) in THF (6 ml) was stirred at RT overnight. The solution was adsorbed onto silica gel and purified by ISCO chromatography (10 to 30% EtOAc:heptane) to afford 95 mg (77%) of the title compound as a yellow solid. 1H NMR (400 MHz, DMSO-d6): δ 6.89 (s, 2 H), 8.05 (s, 1 H).
後処理
- custompurified by ISCO chromatography (10 to 30% EtOAc:heptane)
出典と根拠
- ORDレコード
- ord-a725ace4fc094a08b3a9de8c26ac2396
- 出典データセット
- uspto-grants-2013_02
- 特許番号
- US08378104B2
反応ノート
読み込み中…