Ammonium Hydroxide → 2-(Trifluoromethyl)-[1,2,4]triazolo[1,5-a]pyrazine
反応式
[F:1][C:2]([F:14])([F:13])[C:3](=[N:11]O)[NH:4][C:5]1[CH:10]=[N:9][CH:8]=[CH:7][N:6]=1.[OH-].[NH4+]>>[F:1][C:2]([F:14])([F:13])[C:3]1[N:4]=[C:5]2[CH:10]=[N:9][CH:8]=[CH:7][N:6]2[N:11]=1参加物
3
反応条件
- 温度
- 150 °C
実験手順
A mixture of 2,2,2-trifluoro-N′-hydroxy-N-pyrazin-2-ylethanimidamide (10.5 g, 50.97 mmol, from Step B) and polyphosphoric acid (80 mL) was heated to 150° C. with stirring for 18 h. The solution was added to ice and neutralized by addition of ammonium hydroxide. The dark aqueous solution was extracted three times with ethyl acetate, washed with brine, and dried over anhydrous magnesium sulfate. Concentration followed by flash chromatography (eluting with 50% followed by 100% ethyl acetate/hexane) afforded the title compound as a yellow solid.
後処理
- additionThe solution was added to ice
- extractionThe dark aqueous solution was extracted three times with ethyl acetate
- washwashed with brine
- dry with materialdried over anhydrous magnesium sulfate
- concentrationConcentration
- washfollowed by flash chromatography (eluting with 50% followed by 100% ethyl acetate/hexane)
出典と根拠
- ORDレコード
- ord-96665976fa574224acff39219859ad5d
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08653059B2
反応ノート
読み込み中…