N-Iodosuccinimide → HCID 66779473, 화합물
반응식
[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]=12참가 물질
5
실험 절차
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.
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-d8a13e5a455b4a93afcf2e5a8c070132
- 출처 데이터셋
- uspto-grants-2013_10
- 특허 번호
- US08557816B2
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