反応 #2146694
ord-b5a44cd795b54272b4de73317c71bf2c
反応方程式
反応条件
後処理
- 1温度Then, the mixture was refluxed for 23 hours
- 2温度After the reaction solution was cooled
- 3抽出extracted twice by a salting-out extraction procedure
- 4workup.ADDITIONwith addition of sodium chloride
- 5乾燥The combined chloroform layer was dried over anhydrous magnesium sulfate
- 6その他The resulting crude product was purified by silica gel column chromatography (elution solvent: chloroform/methanol=10/1)
実験手順
1.18 g (corresponding to 3.57 mmol) of 2-[4′-(3″-fluoropropoxy)phenyl]-6-methoxymethoxyimidazo[1,2-a]pyridine was dissolved in 29 mL of isopropyl alcohol, and 0.59 mL of conc. hydrochloric acid was added thereto. Then, the mixture was refluxed for 23 hours. After the reaction solution was cooled, the solution was poured into water, and extracted twice by a salting-out extraction procedure using chloroform with addition of sodium chloride. The combined chloroform layer was dried over anhydrous magnesium sulfate. The resulting crude product was purified by silica gel column chromatography (elution solvent: chloroform/methanol=10/1), to obtain 481 mg (corresponding to 1.68 mmol) of 2-[4′-(3″-fluoropropoxy)phenyl]-6-hydroxyimidazo[1,2-a]pyridine (hereinafter referred to as Compound 2) (FIG. 3, Step 10).