반응 #2146706

반응 방정식

sodium hydrogencarbonate

2-bromo-4′-hydroxyacetophenone

2-amino-5-methoxypyridine

water

→

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

수율 81.6%

용매

acetonitrile

methanol

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
   기타The recovered precipitates
7. 7
   세척were washed with acetonitrile
8. 8
   기타dried under reduced pressure
9. 9
   기타to obtain crude crystals
10. 10
    기타sonicated for 5 minutes by an ultrasonic washing machine
11. 11
    여과The precipitates were filtered
12. 12
    기타recovered from the resulting mixture
13. 13
    세척washed 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 recovered precipitates were washed with acetonitrile, and dried under reduced pressure to obtain crude crystals. The resulting crude crystals were suspended in a mixed solution of 40 mL of water and 40 mL of methanol. The suspension was supplemented with about 20 mL of a saturated sodium hydrogencarbonate solution, and sonicated for 5 minutes by an ultrasonic washing machine. The precipitates were filtered and recovered from the resulting mixture, 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. 1, Step 5).

출처