反応 #2146697

反応方程式

2-bromo-4′-hydroxyacetophenone

2-amino-5-iodopyridine

→

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

収率 78.0%

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
   その他sonicated for 5 minutes
9. 9
   その他Precipitates
10. 10
    ろ過were filtered
11. 11
    その他recovered from the resulting mixture
12. 12
    洗浄sufficiently washed with water
13. 13
    その他dried under reduced pressure

実験手順

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).

出典