Dimethylformamide → 6-chloropyrazine-2-carboxamide
反応式
Cl[C:2]1[CH:7]=[N:6][CH:5]=[C:4]([Cl:8])[N:3]=1.[C-]#N.[K+].C[N:13]([CH:15]=[O:16])C>O>[Cl:8][C:4]1[N:3]=[C:2]([C:15]([NH2:13])=[O:16])[CH:7]=[N:6][CH:5]=1参加物
5
反応条件
- 温度
- 100 °C
実験手順
To a solution of 2,6-dichloropyrazine (50 mg, 0.34 mmol) in DMF (1 mL) was added a solution of potassium cyanide (24 mg, 0.37 mmol) in H2O (1 mL). After stirring for 3 h at 100° C., the reaction mixture was cooled to r.t., poured into H2O (10 mL) and extracted with EtOAc three times. The combined organic layer was dried over MgSO4, filtered and concentrated. The crude product was purified by column chromatography (silica gel, EtOAc:Hexane, 3:7) to give 15 mg of the desired product. Yield: 32%.
後処理
- temperaturethe reaction mixture was cooled to r.t.
- extractionextracted with EtOAc three times
- dry with materialThe combined organic layer was dried over MgSO4
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by column chromatography (silica gel, EtOAc:Hexane, 3:7)
出典と根拠
- ORDレコード
- ord-9e0f0398cae6462da726ec20f7bfbc89
- 出典データセット
- uspto-grants-2009_10
- 特許番号
- US07601742B2
反応ノート
読み込み中…