Methanol → Methyl 6-(ethylamino)pyridine-3-carboxylate
反応式
[CH2:1]([NH:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([OH:10])=[O:9])=[CH:6][N:5]=1)[CH3:2].OS(O)(=O)=O.[CH3:18]O>>[CH2:1]([NH:3][C:4]1[CH:12]=[CH:11][C:7]([C:8]([O:10][CH3:18])=[O:9])=[CH:6][N:5]=1)[CH3:2]参加物
4
実験手順
A suspension of 6-(ethylamino)nicotinic acid (50 g, 0.3 mol) in methanol (500 ml) was treated with concentrated H2SO4 (30 mml). The reaction was heated at reflux for 18 hours. The reaction mixture was then evaporated, poured into ice water (1 L) and adjusted to pH 8 with solid sodium hydrogen carbonate (foaming). The aqueous mixture was extracted with ethyl acetate (3×300 ml) and the organic layers combined, dried (MgSO4) and evaporated to give methyl 6-(ethylamino)nicotinoate as an off-white solid (45.5 g, 84%).
後処理
- temperatureThe reaction was heated
- temperatureat reflux for 18 hours
- customThe reaction mixture was then evaporated
- additionpoured into ice water (1 L)
- extractionThe aqueous mixture was extracted with ethyl acetate (3×300 ml)
- dry with materialdried (MgSO4)
- customevaporated
出典と根拠
- ORDレコード
- ord-402de9e8ffee45aa8dc1872846c35589
- 出典データセット
- uspto-grants-2001_11
- 特許番号
- US06313148B1
反応ノート
読み込み中…