Реакция #1960535

Уравнение реакции

2-bromo-4′-hydroxyacetophenone

2-amino-5-bromopyridine

→

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

Выход 83.2%

Растворители

acetonitrile

Условия реакции

Обработка

1. 1
   ДругоеAfter the completion of the reaction
2. 2
   Температураthe reaction solution was cooled down to room temperature
3. 3
   Другоеprecipitates
4. 4
   Фильтрацияwere filtered
5. 5
   Другоеrecovered
6. 6
   ПромывкаThe precipitates were washed with acetonitrile
7. 7
   Другоеdried under reduced pressure
8. 8
   workup.ADDITIONThen, about 25 mL of a saturated sodium hydrogencarbonate solution was added
9. 9
   Другоеthe mixture was sonicated for 5 minutes
10. 10
    ДругоеPrecipitates
11. 11
    Фильтрацияwere filtered
12. 12
    Другоеrecovered from the resulting mixture
13. 13
    Промывкаsufficiently washed with water
14. 14
    Другоеdried under reduced pressure

Методика

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. 1-3, Step 2).

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