Formic Acid → N-(5-fluoropyridin-2-ylmethyl)-formamide
反応式
[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][NH2:9])=[N:6][CH:7]=1.[CH:10](O)=[O:11].[OH-].[NH4+]>O>[F:1][C:2]1[CH:3]=[CH:4][C:5]([CH2:8][NH:9][CH:10]=[O:11])=[N:6][CH:7]=1参加物
5
実験手順
In a round-bottomed flask, (5-fluoro-pyridin-2-yl)methylamine (557 mg, 4.42 mmol) was dissolved in 88% formic acid (3.6 ml, 82.6 mmol). The brown solution was stirred at reflux in an oil bath overnight. The reaction mixture was cooled to 0° C. and adjusted carefully to pH=9 by addition of 25% aqueous ammonium hydroxide. The mixture was diluted with water and the aqueous layer was extracted with dichloromethane (3×). The organic layers were combined, dried over sodium sulfate, filtered and concentrated to give 614 mg (90%) of N-(5-fluoro-pyridin-2-ylmethyl)-formamide as a brown oil which was used without further purification.
後処理
- temperatureat reflux in an oil bath overnight
- extractionthe aqueous layer was extracted with dichloromethane (3×)
- dry with materialdried over sodium sulfate
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-dcaa0bd1275549859f05e0b2c3636d5b
- 出典データセット
- uspto-grants-2014_02
- 特許番号
- US08658646B2
反応ノート
読み込み中…