Ethanol → Ethyl 2-aminopyridine-3-carboxylate
反応式
[NH2:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=[O:5].[CH3:11][CH2:12]O>S(=O)(=O)(O)O>[CH2:11]([O:5][C:4](=[O:6])[C:3]1[CH:7]=[CH:8][CH:9]=[N:10][C:2]=1[NH2:1])[CH3:12]参加物
4
実験手順
A solution of 2-aminonicotinic acid (2.0 g, 14.4 mmol) in anhydrous EtOH (70 mL) and concentrated sulfuric acid (14 mL) was heated to reflux for 16 h. The solution was concentrated under reduced pressure, neutralized with saturated aqueous Na2CO3 (50 mL) and extracted with CH2Cl2 (3×50 mL). The combined organic phases were dried (MgSO4), filtered and concentrated to give 2-aminonicotinic acid ethyl ester as a yellow solid (1.74 g, 74%). 1H NMR (CDCl3) δ 1.40 (t, 3H, J=6.0 Hz), 4.34 (q, 2H, J=7.0 Hz), 6.41 (br s, 2H (NH2)), 6.63 (m, 1H), 8.14 (d, 1H, J=7.8 Hz), 8.22 (s, 1H).
後処理
- temperatureto reflux for 16 h
- concentrationThe solution was concentrated under reduced pressure
- extractionextracted with CH2Cl2 (3×50 mL)
- dry with materialThe combined organic phases were dried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
出典と根拠
- ORDレコード
- ord-4cc2c5bab2ba4ae7a526bb2725f4a01a
- 出典データセット
- uspto-grants-2006_08
- 特許番号
- US07091217B2
反応ノート
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