Water → 5-Bromo-2-(tetrahydro-2H-pyran-4-yloxy)pyridine
反応式
[O:1]1[CH2:6][CH2:5][CH:4]([OH:7])[CH2:3][CH2:2]1.[H-].[Na+].[Br:10][C:11]1[CH:12]=[CH:13][C:14](Cl)=[N:15][CH:16]=1.O>CN(C=O)C>[Br:10][C:11]1[CH:12]=[CH:13][C:14]([O:7][CH:4]2[CH2:5][CH2:6][O:1][CH2:2][CH2:3]2)=[N:15][CH:16]=1参加物
6
反応条件
- 温度
- 0 °C
実験手順
tetrahydro-2H-pyran-4-ol (850 mg, 8.32 mmol) was dissolved in DMF (10 mL), cooled to 0° C., NaH (500 mg, 10.4 mmol) was added and stirred for 45 minutes at room temperature, then 5-bromo-2-chloropyridine (2 g, 10.4 mmol) was added and the mixture was stirred overnight at 60° C. The mixture was poured into water, extracted by EA, the organic layer was washed by brine, dried over Na2SO4, concentrated and purified by flash chromatography, gave 1.7 g white solid. MS: (m/z): 258 (M−H)+, 260 (M+H)+
後処理
- stirringthe mixture was stirred overnight at 60° C
- extractionextracted by EA
- washthe organic layer was washed by brine
- dry with materialdried over Na2SO4
- concentrationconcentrated
- custompurified by flash chromatography
出典と根拠
- ORDレコード
- ord-7694a110ba134784a421258096b9983e
- 出典データセット
- uspto-grants-2016_09
- 特許番号
- US09434726B2
反応ノート
読み込み中…