Dichloromethane → 5-Bromo-6-methoxy-3-pyridineacetonitrile
反応式
[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]参加物
6
反応条件
- 温度
- 50 °C
実験手順
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).
後処理
- 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)
出典と根拠
- ORDレコード
- ord-5aa2b8b6860644b6bd34ff05eabadaa9
- 出典データセット
- uspto-grants-2016_06
- 特許番号
- US09365576B2
反応ノート
読み込み中…