1,2-Dichloroethane → 2-Amino-N-methylpyridine-3-carboxamide
반응식
[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]참가 물질
7
실험 절차
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%).
후처리
- 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)
출처 및 근거
- ORD 기록
- ord-b6aec88fc52e4d6880e8b85dcf8f4ab0
- 출처 데이터셋
- uspto-grants-2013_08
- 특허 번호
- US08501763B2
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