반응 #2146697

반응 방정식

2-bromo-4′-hydroxyacetophenone

2-amino-5-iodopyridine

→

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

수율 78.0%

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
   기타sonicated for 5 minutes
9. 9
   기타Precipitates
10. 10
    여과were filtered
11. 11
    기타recovered from the resulting mixture
12. 12
    세척sufficiently washed with water
13. 13
    기타dried under reduced pressure

실험 절차

441 mg (corresponding to 2.0 mmol) of 2-bromo-4′-hydroxyacetophenone and 449 mg (corresponding to 2.0 mmol) of 2-amino-5-iodopyridine were dissolved in 15 mL of acetonitrile. The resulting solution was refluxed in an oil bath at 110° C. for 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 10 mL of water and 10 mL of methanol, and then supplemented with about 10 mL of a saturated sodium hydrogencarbonate solution and sonicated for 5 minutes using an ultrasonic washing machine. Precipitates were filtered and recovered from the resulting mixture, sufficiently washed with water, and dried under reduced pressure, to obtain 526 mg (corresponding to 1.56 mmol) of 2-(4′-hydroxyphenyl)-6-iodoimidazo[1,2-a]pyridine (FIG. 5, Step 2).

출처