반응 #2146686

반응 방정식

2-bromo-4′-hydroxyacetophenone

2-amino-5-methoxypyridine

→

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

수율 81.6%

용매

acetonitrile

반응 조건

후처리

1. 1
   기타After the completion of the reaction
2. 2
   온도the reaction solution was cooled down to room temperature
3. 3
   기타precipitates
4. 4
   여과were filtered
5. 5
   기타recovered
6. 6
   세척The precipitates were washed with acetonitrile
7. 7
   기타dried under reduced pressure
8. 8
   workup.ADDITIONThen, about 20 mL of a saturated sodium hydrogencarbonate solution was added
9. 9
   기타the mixture was sonicated for 5 minutes
10. 10
    기타Precipitates
11. 11
    여과were filtered
12. 12
    기타recovered from the resulting mixture
13. 13
    세척sufficiently washed with water
14. 14
    기타dried under reduced pressure

실험 절차

2.15 g (corresponding to 10.0 mmol) of 2-bromo-4′-hydroxyacetophenone and 1.25 g (corresponding to 10.0 mmol) of 2-amino-5-methoxypyridine were dissolved in 50 mL, of acetonitrile. The resulting solution was refluxed in an oil bath at 90° C. for 3.5 hours. After the completion of the reaction, the reaction solution was cooled down to room temperature, and precipitates were filtered and recovered. The precipitates were washed with acetonitrile and dried under reduced pressure. The resulting crude crystals were suspended in a mixed solution of 40 mL of water and 40 mL of methanol. Then, about 20 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was sonicated for 5 minutes using a ultrasonic washing machine. Precipitates were filtered and recovered from the resulting mixture, sufficiently washed with water, and dried under reduced pressure, to obtain 1.96 g (corresponding to 8.16 mmol) of 2-(4′-hydroxyphenyl)-6-methoxyimidazo[1,2-a]pyridine (FIG. 2, Step 5).

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