Sulfuric Acid → 3-Amino-6-(trifluoromethyl)picolinamide
反応式
[NH2:1][C:2]1[CH:3]=[CH:4][C:5]([C:10]([F:13])([F:12])[F:11])=[N:6][C:7]=1[C:8]#[N:9].S(=O)(=O)(O)[OH:15]>>[NH2:1][C:2]1[C:7]([C:8]([NH2:9])=[O:15])=[N:6][C:5]([C:10]([F:13])([F:11])[F:12])=[CH:4][CH:3]=1参加物
3
反応条件
- 温度
- 70 °C
実験手順
7 g (0.0374 mol, 1 eq) of 5-amino-6-cyano-2-(trifluoromethyl)pyridine dissolved in 106 ml of 90% sulfuric acid was and heated at 70° C. for 3 h. The reaction mixture was cooled to RT and quenched with ice water and extracted with ethyl acetate. The organic layer was washed with brine and concentrated. The solid product obtained was washed with to get 6.8 g (89.47%) of off white solid. 1H NMR (CDCl3, 400 MHz) 5.5 (1H, bs), 7.1 (1H, d), 7.53 (1H, d), 7.80 (1H, bs). MS 206 (M+H)+.
後処理
- temperatureThe reaction mixture was cooled to RT
- customquenched with ice water
- extractionextracted with ethyl acetate
- washThe organic layer was washed with brine
- concentrationconcentrated
- customThe solid product obtained
- washwas washed with
- customto get 6.8 g (89.47%) of off white solid
出典と根拠
- ORDレコード
- ord-2f4895a0831546f3b316c1377eb2d52b
- 出典データセット
- uspto-grants-2011_07
- 特許番号
- US07985861B2
反応ノート
読み込み中…