Dimethylformamide → 2-Iodo-5-propoxypyridine
反応式
I[CH2:2][CH2:3][CH3:4].[I:5][C:6]1[N:11]=[CH:10][C:9]([OH:12])=[CH:8][CH:7]=1.C(=O)(O)[O-].[K+].CN(C=O)C>C(Cl)Cl.O>[I:5][C:6]1[CH:7]=[CH:8][C:9]([O:12][CH2:2][CH2:3][CH3:4])=[CH:10][N:11]=1参加物
7
反応条件
- 温度
- 80 °C
実験手順
Iodopropane (0.18 mL, 1.8 mmol) was added dropwise to a mixture comprising 6-iodopyridin-3-ol (0.32 g, 1.14 mmol), potassium bicarbonate (0.23 g, 1.7 mmol) and DMF (2 mL). The mixture was heated at 80° C. for 1 hour, cooled and diluted with methylene chloride and water. The aqueous layer was separated and extracted with methylene chloride (20 mL). The combined organic layers were washed with water 30 mL, dried (MgSO4) and concentrated under reduced pressure to provide 2-iodo-5-propoxypyridine. MS (ESI); Calculated for C8H10NIO, 266.1, Found (MH+): 222.
後処理
- temperaturecooled
- customThe aqueous layer was separated
- extractionextracted with methylene chloride (20 mL)
- washThe combined organic layers were washed with water 30 mL
- dry with materialdried (MgSO4)
- concentrationconcentrated under reduced pressure
出典と根拠
- ORDレコード
- ord-83809f9e206d4f349bf62a97ce46f2c2
- 出典データセット
- uspto-grants-2000_11
- 特許番号
- US06150379
反応ノート
読み込み中…