Реакция #2146706

Уравнение реакции

sodium hydrogencarbonate

2-bromo-4′-hydroxyacetophenone

2-amino-5-methoxypyridine

water

→

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

Выход 81.6%

Растворители

acetonitrile

methanol

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
   ДругоеThe recovered precipitates
7. 7
   Промывкаwere washed with acetonitrile
8. 8
   Другоеdried under reduced pressure
9. 9
   Другоеto obtain crude crystals
10. 10
    Другоеsonicated for 5 minutes by an ultrasonic washing machine
11. 11
    ФильтрацияThe precipitates were filtered
12. 12
    Другоеrecovered from the resulting mixture
13. 13
    Промывкаwashed with water
14. 14
    Другоеdried under reduced pressure

Методика

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).

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