Hydrochloric Acid → 6-(Difluoromethoxy)pyridin-3-amine
反応式
[F:1][CH:2]([F:13])[O:3][C:4]1[CH:9]=[CH:8][C:7]([N+:10]([O-])=O)=[CH:6][N:5]=1.Cl>C(O)C.O.[Fe]>[F:13][CH:2]([F:1])[O:3][C:4]1[N:5]=[CH:6][C:7]([NH2:10])=[CH:8][CH:9]=1参加物
6
実験手順
2-Difluoromethoxy-5-nitro-pyridine obtained in Step A (1.6 g) was treated with iron (5 g) and concentrated hydrochloric acid (0.23 ml) in ethanol (15 ml) and water (2.5 ml) at 80° C. for 20 minutes. Filtration over Celite® and evaporation of the solvent afforded 6-difluoromethoxy-pyridin-3-yl-amine (1.4 g) as an orange solid. 1H NMR (400 MHz, CDCl3) 3.51 (br s, 2H), 6.89 (d, 1H), 7.23 (d, 1H), 7.44 (dd, 1H), 7.80 (d, 1H).
後処理
- filtrationFiltration
- customover Celite® and evaporation of the solvent
出典と根拠
- ORDレコード
- ord-07561f2678fc4369b4745da9f722f65b
- 出典データセット
- uspto-grants-2012_06
- 特許番号
- US08193362B2
反応ノート
読み込み中…