反応 #2146686

反応方程式

2-bromo-4′-hydroxyacetophenone

2-amino-5-methoxypyridine

→

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

収率 81.6%

溶媒

acetonitrile

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
   洗浄The precipitates were washed with acetonitrile
7. 7
   その他dried under reduced pressure
8. 8
   workup.ADDITIONThen, about 20 mL of a saturated sodium hydrogencarbonate solution was added
9. 9
   その他the mixture was sonicated for 5 minutes
10. 10
    その他Precipitates
11. 11
    ろ過were filtered
12. 12
    その他recovered from the resulting mixture
13. 13
    洗浄sufficiently 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 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).

出典