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2-[4′-(3″-fluoropropoxy)phenyl]-6-methoxymethoxyimidazo[1,2-a]pyridine

hydrochloric acid

water

→

2-[4′-(3″-fluoropropoxy)phenyl]-6-hydroxyimidazo[1,2-a]pyridine

수율 47.1%

용매

isopropyl alcohol

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후처리

1. 1
   온도Then, the mixture was refluxed for 23 hours
2. 2
   온도After the reaction solution was cooled
3. 3
   추출extracted twice by a salting-out extraction procedure
4. 4
   workup.ADDITIONwith addition of sodium chloride
5. 5
   건조The combined chloroform layer was dried over anhydrous magnesium sulfate
6. 6
   기타The resulting crude product was purified by silica gel column chromatography (elution solvent: chloroform/methanol=10/1)

실험 절차

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).

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