تفاعل #2146686

معادلة التفاعل

2-bromo-4′-hydroxyacetophenone

2-amino-5-methoxypyridine

→

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

المردود 81.6%

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
   workup.ADDITIONThen, about 20 mL of a saturated sodium hydrogencarbonate solution was added
9. 9
   أخرىthe mixture was sonicated for 5 minutes
10. 10
    أخرىPrecipitates
11. 11
    ترشيحwere filtered
12. 12
    أخرىrecovered from the resulting mixture
13. 13
    غسيلsufficiently washed 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 precipitates were washed with acetonitrile and dried under reduced pressure. The resulting crude crystals were suspended in a mixed solution of 40 mL of water and 40 mL of methanol. Then, about 20 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was sonicated for 5 minutes using a ultrasonic washing machine. Precipitates were filtered and recovered from the resulting mixture, sufficiently 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. 2, Step 5).

المصدر