Ammonia → 6-Bromopyridine-2-carboxamide
反応式
[Br:1][C:2]1[N:7]=[C:6]([C:8]([OH:10])=O)[CH:5]=[CH:4][CH:3]=1.[NH3:11]>S(Cl)(Cl)=O.O1CCOCC1>[Br:1][C:2]1[N:7]=[C:6]([C:8]([NH2:11])=[O:10])[CH:5]=[CH:4][CH:3]=1参加物
5
反応条件
- 温度
- 70 °C
実験手順
6-Bromopicolinic acid (1000 mg, 4.95 mmol) was suspended in thionyl chloride (15 mL) and heated at 70° C. for 5 h. The reaction was cooled to room temperature and the volatiles were condensed under reduced pressure. A solution of ammonia (2M in dioxane (15 mL) was added to the residue and then the solvents were removed under reduced pressure. The crude residue was purified by MPLC with a gradient of 0 to 20% MeOH/dichloromethane to give 6-Bromo-pyridine-2-carboxylic acid amide as a white powder (555 mg, 45%). MS ES (MH+=201.0/203.0).
後処理
- temperatureThe reaction was cooled to room temperature
- customcondensed under reduced pressure
- customthe solvents were removed under reduced pressure
- customThe crude residue was purified by MPLC with a gradient of 0 to 20% MeOH/dichloromethane
出典と根拠
- ORDレコード
- ord-c44d8a796e344fa9ab518435508d9ef8
- 出典データセット
- uspto-grants-2008_09
- 特許番号
- US07420066B2
反応ノート
読み込み中…