1,2-Dichloroethane → 2-Amino-N-methylpyridine-3-carboxamide
反応式
[NH2:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([OH:6])=O.Cl.CN.C(Cl)CCl.C1C=CC2N(O)N=[N:24][C:22]=2C=1.CCN(C(C)C)C(C)C>CN(C=O)C>[NH2:1][C:2]1[N:10]=[CH:9][CH:8]=[CH:7][C:3]=1[C:4]([NH:24][CH3:22])=[O:6]参加物
7
実験手順
To the mixture of 2-aminonicotinic acid (2.0 g, 14.5 mmol), methylamine hydrogen chloride (1.47 g, 1.5 eq), EDC (4.49 g, 1.5 eq), HOBt (2.35 g, 1.2 eq) in DMF (20 mL) was added DIEA (7.6 mL, 3.0 eq). The mixture was stirred at room temperature overnight. The crude was concentrated and dissolved in EtOAc. It was washed with saturated NaHCO3. The solvent was removed and the crude was purified by silica gel chromatography (0%˜20% MeOH/DCM) to obtain the desired product 2-amino-N-methylnicotinamide (2.16 g, isolated yield ˜98%).
後処理
- concentrationThe crude was concentrated
- dissolutiondissolved in EtOAc
- washIt was washed with saturated NaHCO3
- customThe solvent was removed
- customthe crude was purified by silica gel chromatography (0%˜20% MeOH/DCM)
出典と根拠
- ORDレコード
- ord-b6aec88fc52e4d6880e8b85dcf8f4ab0
- 出典データセット
- uspto-grants-2013_08
- 特許番号
- US08501763B2
反応ノート
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