تفاعل #2146706

معادلة التفاعل

sodium hydrogencarbonate

2-bromo-4′-hydroxyacetophenone

2-amino-5-methoxypyridine

water

→

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

المردود 81.6%

المذيبات

acetonitrile

methanol

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
   أخرىThe recovered precipitates
7. 7
   غسيلwere washed with acetonitrile
8. 8
   أخرىdried under reduced pressure
9. 9
   أخرىto obtain crude crystals
10. 10
    أخرىsonicated for 5 minutes by an ultrasonic washing machine
11. 11
    ترشيحThe precipitates were filtered
12. 12
    أخرىrecovered from the resulting mixture
13. 13
    غسيلwashed with water
14. 14
    أخرىdried under reduced pressure

الإجراء التجريبي

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).

المصدر