Reaktion #2146697

Reaktionsgleichung

2-bromo-4′-hydroxyacetophenone

2-amino-5-iodopyridine

→

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

Ausbeute 78.0%

Lösungsmittel

acetonitrile

Reaktionsbedingungen

Aufarbeitung

1. 1
   SonstigeAfter the completion of the reaction
2. 2
   Temperaturthe reaction solution was cooled down to room temperature
3. 3
   Sonstigeprecipitates
4. 4
   Filtrationwere filtered
5. 5
   Sonstigerecovered
6. 6
   WaschenThe precipitates were washed with acetonitrile
7. 7
   Sonstigedried under reduced pressure
8. 8
   Sonstigesonicated for 5 minutes
9. 9
   SonstigePrecipitates
10. 10
    Filtrationwere filtered
11. 11
    Sonstigerecovered from the resulting mixture
12. 12
    Waschensufficiently washed with water
13. 13
    Sonstigedried under reduced pressure

Vorschrift

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).

Quelle