Dimethylamine → N,N-dimethyl-5-nitropyridin-2-amine
반응식
Cl[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1.[CH3:11][NH:12][CH3:13]>CO>[CH3:11][N:12]([CH3:13])[C:2]1[CH:7]=[CH:6][C:5]([N+:8]([O-:10])=[O:9])=[CH:4][N:3]=1참가 물질
4
실험 절차
To 0.314 g (1.99 mmol) of 2-chloro-5-nitropyridine in MeOH (1 mL) was added 5 mL of dimethylamine (2M solution in MeOH) at 0° C. and the mixture was warmed to room temperature. The reaction mixture was concentrated and extracted with EtOAc. The organic layer was washed successively with sat. NaHCO3 solution and brine, dried (Na2SO4), and concentrated to give 0.313 g (94% yield) of 2-dimethylamino-5-nitropyridine as an orange powder: 1H NMR (CDCl3) δ9.06 (d, J=2.7 Hz, 1H), 8.20 (dd, J=9.5, 2.7 Hz, 1H), 6.46 (dd, J=9.5, 0.4 Hz, 1H), 3.23 (s, 6H); LCMS (APCI+) m/z: 168 (MH+, 100%).
후처리
- concentrationThe reaction mixture was concentrated
- extractionextracted with EtOAc
- washThe organic layer was washed successively with sat. NaHCO3 solution and brine
- dry with materialdried (Na2SO4)
- concentrationconcentrated
출처 및 근거
- ORD 기록
- ord-504f0d6541004dee8daa2c596cc37001
- 출처 데이터셋
- uspto-grants-2013_07
- 특허 번호
- US08486939B2
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