Methylamine → N-Methyl-5-(trifluoromethyl)pyridin-2-amine
反応式
Cl[C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][N:3]=1.[CH3:12][N:13]1CCCC1=O.CN>O>[CH3:12][NH:13][C:2]1[CH:7]=[CH:6][C:5]([C:8]([F:11])([F:10])[F:9])=[CH:4][N:3]=1参加物
5
実験手順
To a mixture of 2-chloro-5-trifluoromethylpyridine (18.2) and N-methylpyrrolidone (100 ml), 40% of aqueous methylamine solution (23.3 g) was added, and stirred at room temperature for 3 hours. Water was poured thereinto, and extracted with ethyl acetate 3 times. The combined organic layer was dried over magnesium sulfate, and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography to give 17.3 g of N-methyl-(5-trifluoromethyl-pyridin-2-yl)-amine.
後処理
- additionwas added
- extractionextracted with ethyl acetate 3 times
- dry with materialThe combined organic layer was dried over magnesium sulfate
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-33d6185e5043400285a972d6e13d7f9b
- 出典データセット
- uspto-grants-2016_03
- 特許番号
- US09278983B2
反応ノート
読み込み中…