反応 #2146706

反応方程式

sodium hydrogencarbonate

2-bromo-4′-hydroxyacetophenone

2-amino-5-methoxypyridine

water

→

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

収率 81.6%

溶媒

acetonitrile

methanol

反応条件

後処理

1. 1
   その他After the completion of the reaction
2. 2
   温度the reaction solution was cooled down to room temperature
3. 3
   その他precipitates
4. 4
   ろ過were filtered
5. 5
   その他recovered
6. 6
   その他The recovered precipitates
7. 7
   洗浄were washed with acetonitrile
8. 8
   その他dried under reduced pressure
9. 9
   その他to obtain crude crystals
10. 10
    その他sonicated for 5 minutes by an ultrasonic washing machine
11. 11
    ろ過The precipitates were filtered
12. 12
    その他recovered from the resulting mixture
13. 13
    洗浄washed with water
14. 14
    その他dried under reduced pressure

実験手順

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).

出典