Iodine → HCID 12786936, 화합물
반응식
[C:1]([C:4]1[CH:9]=[CH:8][CH:7]=[C:6]([Br:10])[N:5]=1)(=[O:3])[CH3:2].[I:11]I.C(O)(C)C.[N:17]1[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=1>>[I-:11].[Br:10][C:6]1[N:5]=[C:4]([C:1](=[O:3])[CH2:2][N+:17]2[CH:22]=[CH:21][CH:20]=[CH:19][CH:18]=2)[CH:9]=[CH:8][CH:7]=1참가 물질
5
실험 절차
To a stirred solution of 2-acetyl-6-bromopyridine (100 g; 0.5 mole) in 600 mL pyridine was added iodine (127 g; 0.5 mole). The mixture was heated on a steam bath for 45 minutes, and the product crystallized on cooling. The solid was filtered and the light yellow crystalline cake was rinsed twice with methylene chloride. After drying, 183 g (90%) was obtained. MP 176°-178° C.; silica gel TLC system: 95acetone: 5 isopropanol.
후처리
- temperatureThe mixture was heated on a steam bath for 45 minutes
- customthe product crystallized
- temperatureon cooling
- filtrationThe solid was filtered
- washthe light yellow crystalline cake was rinsed twice with methylene chloride
- customAfter drying
- custom183 g (90%) was obtained
출처 및 근거
- ORD 기록
- ord-fdae55a513b742c28bcefa581f5a4824
- 출처 데이터셋
- uspto-grants-1998_01
- 특허 번호
- US05707603
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