تفاعل #2146697

معادلة التفاعل

2-bromo-4′-hydroxyacetophenone

2-amino-5-iodopyridine

→

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

المردود 78.0%

المذيبات

acetonitrile

ظروف التفاعل

المعالجة

1. 1
   أخرىAfter the completion of the reaction
2. 2
   درجة الحرارةthe reaction solution was cooled down to room temperature
3. 3
   أخرىprecipitates
4. 4
   ترشيحwere filtered
5. 5
   أخرىrecovered
6. 6
   غسيلThe precipitates were washed with acetonitrile
7. 7
   أخرىdried under reduced pressure
8. 8
   أخرىsonicated for 5 minutes
9. 9
   أخرىPrecipitates
10. 10
    ترشيحwere filtered
11. 11
    أخرىrecovered from the resulting mixture
12. 12
    غسيلsufficiently washed with water
13. 13
    أخرىdried under reduced pressure

الإجراء التجريبي

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).

المصدر