반응 #2146692

반응 방정식

4′-benzoyloxy-2-bromoacetophenone

2-amino-5-methoxypyridine

sodium hydrogencarbonate

→

2-(4′-benzoyloxyphenyl)-6-methoxyimidazo[1,2-a]pyridine

수율 70.7%

용매

ethanol

반응 조건

후처리

1. 1
   온도The resulting solution was refluxed for 2 hours
2. 2
   온도After the reaction solution was cooled
3. 3
   기타The resulting reaction mixture
4. 4
   온도was further refluxed for 4 hours
5. 5
   기타After the completion of the reaction
6. 6
   농축the solvent was concentrated under reduced pressure
7. 7
   workup.DISSOLUTIONThe resulting residue was dissolved in chloroform
8. 8
   세척washed with water
9. 9
   건조After the chloroform layer was dried over anhydrous sodium sulfate
10. 10
    workup.DISTILLATIONthe solvent was distilled off
11. 11
    기타The resulting crude product was purified by silica gel column chromatography (elution solvent: chloroform/ethyl acetate=20/1)

실험 절차

13.33 g (corresponding to 43.68 mmol) of 4′-benzoyloxy-2-bromoacetophenone and 5.67 g (corresponding to 45.67 mmol) of 2-amino-5-methoxypyridine were dissolved in 481 mL of ethanol. The resulting solution was refluxed for 2 hours. After the reaction solution was cooled, 6.64 g (corresponding to 79.09 mmol) of sodium hydrogencarbonate was added thereto. The resulting reaction mixture was further refluxed for 4 hours. After the completion of the reaction, the solvent was concentrated under reduced pressure. The resulting residue was dissolved in chloroform and then washed with water. After the chloroform layer was dried over anhydrous sodium sulfate, the solvent was distilled off. The resulting crude product was purified by silica gel column chromatography (elution solvent: chloroform/ethyl acetate=20/1) to obtain 10.20 g (corresponding to 30.87 mmol) of 2-(4′-benzoyloxyphenyl)-6-methoxyimidazo[1,2-a]pyridine (FIG. 3, Step 5).

출처