Dichloromethane → 5-Bromo-6-methoxy-3-pyridineacetonitrile
반응식
[Br:1][C:2]1[C:3]([O:10][CH3:11])=[N:4][CH:5]=[C:6]([CH2:8]Br)[CH:7]=1.[C-:12]#[N:13].[Na+].C(Cl)Cl.C([O-])(O)=O.[Na+]>O>[Br:1][C:2]1[CH:7]=[C:6]([CH2:8][C:12]#[N:13])[CH:5]=[N:4][C:3]=1[O:10][CH3:11]참가 물질
6
반응 조건
- 온도
- 50 °C
실험 절차
To a suspension of 3-bromo-5-bromomethyl-2-methoxy-pyridine (Step AM2) (3.9 g, 14.0 mmol) in H2O was added NaCN (750 mg, 15.3 mmol) and the mixture was stirred at 50° C. for 1.5 h. CH2Cl2 and a saturated aqueous solution of NaHCO3 were added and the phases were separated. The organic layer was washed with H2O and brine, dried (MgSO4), filtered and concentrated. The crude product was purified by silica gel column chromatography (heptane/EtOAc, 80:20→0:100). tR: 0.88 min (LC-MS 1).
후처리
- customthe phases were separated
- washThe organic layer was washed with H2O and brine
- dry with materialdried (MgSO4)
- filtrationfiltered
- concentrationconcentrated
- customThe crude product was purified by silica gel column chromatography (heptane/EtOAc, 80:20→0:100)
출처 및 근거
- ORD 기록
- ord-5aa2b8b6860644b6bd34ff05eabadaa9
- 출처 데이터셋
- uspto-grants-2016_06
- 특허 번호
- US09365576B2
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