反応 #1960538

反応方程式

2-bromo-4′-hydroxyacetophenone

2-amino-5-bromopyridine

→

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

収率 83.2%

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 25 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 1.74 g (corresponding to 10.0 mmol) of 2-amino-5-bromopyridine were dissolved in 50 mL of acetonitrile. The resulting solution was refluxed in an oil bath at 105° C. for 6 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 20 mL of water and 20 mL of methanol. Then, about 25 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was 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 2.41 g (corresponding to 8.32 mmol) of 6-bromo-2-(4′-hydroxyphenyl)imidazo[1,2-a]pyridine (FIG. 1-4, Step 2).

出典