Réaction #2146702
ord-5183adf1a6b141d4b45c5723979a1ad1
Équation de réaction
Réactifs
Solvants
Conditions de réaction
Traitement
- 1AutreAfter the completion of the reaction
- 2Températurethe reaction solution was cooled down to room temperature
- 3Autreprecipitates
- 4Filtrationwere filtered
- 5Autrerecovered
- 6LavageThe precipitates were washed with acetonitrile
- 7Autredried under reduced pressure
- 8Autresonicated for 5 minutes
- 9AutrePrecipitates
- 10Filtrationwere filtered
- 11Autrerecovered from the resulting mixture
- 12Lavagesufficiently washed with water
- 13Autredried under reduced pressure
Mode opératoire
2.15 g (corresponding to 10.0 mmol) of 2-bromo-4′-hydroxyacetophenone and 1.74 g (corresponding to 10.0 mmol) of 2-amino-5-bromopyridine were dissolved in 50 mL of acetonitrile. The resulting solution was refluxed in an oil bath at 105° C. for 6 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 20 mL of water and 20 mL of methanol, and then supplemented with about 25 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 2.41 g (corresponding to 8.32 mmol) of 6-bromo-2-(4′-hydroxyphenyl)imidazo[1,2-a]pyridine (FIG. 8, Step 2).