N-Iodosuccinimide → HCID 66779473、化合物
反応式
[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[CH:8]=[C:9]([Si](C)(C)C)[O:10][C:3]=12.C1C(=O)N([I:22])C(=O)C1.[F-].[K+]>C(#N)C>[Cl:1][C:2]1[CH:7]=[CH:6][N:5]=[C:4]2[CH:8]=[C:9]([I:22])[O:10][C:3]=12参加物
5
実験手順
7-Chloro-2-(trimethylsilyl)furo[3,2-b]pyridine (0.250 g, 1.11 mmol) and NIS (2.49 g, 11.1 mmol) were dissolved in 3 mL of ACN and stirred for 5 minutes. Potassium fluoride (0.0708 g, 1.22 mmol) was added and the reaction was stirred at 50° C. for one hour. The reaction was concentrated, redissolved in ethyl acetate, and washed with saturated sodium thiosulfate, water and brine. The organic layer was dried with sodium sulfate, filtered, and concentrated. The crude material was purified via column chromatography (gradient elution 0-100% EtOAc:Hex) to afford 7-chloro-2-iodofuro[3,2-b]pyridine as a white solid. MS: M+H+=280.2.
後処理
- stirringthe reaction was stirred at 50° C. for one hour
- concentrationThe reaction was concentrated
- dissolutionredissolved in ethyl acetate
- washwashed with saturated sodium thiosulfate, water and brine
- dry with materialThe organic layer was dried with sodium sulfate
- filtrationfiltered
- concentrationconcentrated
- customThe crude material was purified via column chromatography (gradient elution 0-100% EtOAc:Hex)
出典と根拠
- ORDレコード
- ord-c43f9aaff1a744d8a1a892c14b667d8b
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07981891B2
反応ノート
読み込み中…