تفاعل #2146692

معادلة التفاعل

4′-benzoyloxy-2-bromoacetophenone

2-amino-5-methoxypyridine

sodium hydrogencarbonate

→

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

المردود 70.7%

المذيبات

ethanol

ظروف التفاعل

المعالجة

1. 1
   درجة الحرارةThe resulting solution was refluxed for 2 hours
2. 2
   درجة الحرارةAfter the reaction solution was cooled
3. 3
   أخرىThe resulting reaction mixture
4. 4
   درجة الحرارةwas further refluxed for 4 hours
5. 5
   أخرىAfter the completion of the reaction
6. 6
   تركيزthe solvent was concentrated under reduced pressure
7. 7
   workup.DISSOLUTIONThe resulting residue was dissolved in chloroform
8. 8
   غسيلwashed with water
9. 9
   تجفيفAfter the chloroform layer was dried over anhydrous sodium sulfate
10. 10
    workup.DISTILLATIONthe solvent was distilled off
11. 11
    أخرىThe resulting crude product was purified by silica gel column chromatography (elution solvent: chloroform/ethyl acetate=20/1)

الإجراء التجريبي

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).

المصدر