Ethyl Acetate → 5-Bromo-2-(methylsulfinyl)pyridine
反応式
[Br:1][C:2]1[CH:3]=[CH:4][C:5]([S:8][CH3:9])=[N:6][CH:7]=1.C(OCC)(=[O:12])C>O.C(O)(=O)C>[Br:1][C:2]1[CH:3]=[CH:4][C:5]([S:8]([CH3:9])=[O:12])=[N:6][CH:7]=1参加物
5
実験手順
NalO4 (0.52 g) dissolved in water (0.5 mL) was added to a solution of 5-bromo-2-methylsulfanyl-pyridine (0.25 g) in acetic acid (3 mL) at room temperature. The resulting mixture was stirred at room temperature overnight. Then, water and ethyl acetate were added and the mixture was stirred for another 10 min. The organic phase was separated and washed with 10% aqueous Na2S2O3 solution, 10% aqueous K2CO3 solution, and brine. After drying (MgSO4), the solvent was evaporated to afford the title compound. Yield: 0.20 g (72% of theory); Mass spectrum (ESI+): m/z=220/222 (Br) [M+H]+.
後処理
- stirringthe mixture was stirred for another 10 min
- customThe organic phase was separated
- washwashed with 10% aqueous Na2S2O3 solution, 10% aqueous K2CO3 solution, and brine
- dry with materialAfter drying (MgSO4)
- customthe solvent was evaporated
出典と根拠
- ORDレコード
- ord-deb7fa39ccb74c9b86cd34a40cf2f002
- 出典データセット
- uspto-grants-2013_10
- 特許番号
- US08569292B2
反応ノート
読み込み中…