Реакция #2146697

Уравнение реакции

2-bromo-4′-hydroxyacetophenone

2-amino-5-iodopyridine

→

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

Выход 78.0%

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
   Другоеsonicated for 5 minutes
9. 9
   ДругоеPrecipitates
10. 10
    Фильтрацияwere filtered
11. 11
    Другоеrecovered from the resulting mixture
12. 12
    Промывкаsufficiently washed with water
13. 13
    Другоеdried under reduced pressure

Методика

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).

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