Acetyl chloride → HCID 68955615、化合物
反応式
[Br:1][C:2]1[CH:3]=[C:4]([C:8](=[N:10][OH:11])[NH2:9])[CH:5]=[N:6][CH:7]=1.[C:12](Cl)(=O)[CH3:13]>N1C=CC=CC=1.CCOC(C)=O.C([O-])(O)=O.[Na+]>[Br:1][C:2]1[CH:7]=[N:6][CH:5]=[C:4]([C:8]2[N:9]=[C:12]([CH3:13])[O:11][N:10]=2)[CH:3]=1参加物
6
反応条件
- 温度
- 100 °C
実験手順
To a solution of 5-bromo-N′-hydroxypyridine-3-carboximidamide (1.0 eq.) in pyridine was added acetyl chloride (2 eq). The reaction stirred at 100° C. for 1 h and 2 eq of acetyl chloride was added. After 1 h, the mixture was cooled, diluted with EtOAc and aqueous NaHCO3. The organic extracts were washed with aqueous NaHCO3, brine, dried over Na2SO4, filtered and concentrated. Flash chromatography (Hex:EtOAc; 70:30) afforded the title compound as a white solid.
後処理
- waitAfter 1 h
- temperaturethe mixture was cooled
- washThe organic extracts were washed with aqueous NaHCO3, brine
- dry with materialdried over Na2SO4
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-34748353cc7147f18bf80fe0931b3dd7
- 出典データセット
- uspto-grants-2009_01
- 特許番号
- US07482456B2
反応ノート
読み込み中…