6-Methyl-2-nitropyridin-3-ol → 2-Amino-6-methylpyridin-3-ol
反応式
[CH3:1][C:2]1[N:7]=[C:6]([N+:8]([O-])=O)[C:5]([OH:11])=[CH:4][CH:3]=1>[Pd].C(OCC)(=O)C>[NH2:8][C:6]1[C:5]([OH:11])=[CH:4][CH:3]=[C:2]([CH3:1])[N:7]=1参加物
4
実験手順
A mixture of 6-methyl-2-nitro-pyridin-3-ol (18.5 g, 0.120 mmol), 10% palladium on activated carbon (1.35 g), and ethyl acetate (240 mL) was hydrogenated for 3 days. The mixture was filtered through Celite and washed with methanol/ethylacetate (5%). The filtrate and washing were combined and concentrated to give the title compound (14.7 g, 99% yield) as a pale brown solid. 1H NMR (DMSO-d6) δ 9.19 (bs, 1H), 6.73 (d, 1H, J=7.6 Hz), 6.12 (d, 1H, J=7.6 Hz), 5.36 (bs, 2H), 2.15 (s, 3H).
後処理
- filtrationThe mixture was filtered through Celite
- washwashed with methanol/ethylacetate (5%)
- washThe filtrate and washing
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-9ced7b6581684eca95fe4d1a3fb3dbc2
- 出典データセット
- uspto-grants-2005_02
- 特許番号
- US06855722B2
反応ノート
読み込み中…