2-Pyridinamine, 5-iodo- → HCID 71079854, compound

120 mg (corresponding to 0.454 mmol) of 4-(1H-pyrrole-1-yl)phenacylbromide and 99.9 mg (corresponding to 0.454 mmol) of 2-amino-5-iodopyridine were dissolved in 2.0 mL of acetonitrile. The resulting solution was heated under reflux for 2 hours. After the completion of the reaction, the reaction solution was cooled down to room temperature, and precipitates were filtered. 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. Then, about 20 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was sonicated for 20 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 120 mg (corresponding to 0.312 mmol) of 6-iodo-2-[4-(1H-pyrrole-1-yl)phenyl]imidazo[1,2-a]pyridine (FIG. 2, step 2).

1. temperatureThe resulting solution was heated
2. temperatureunder reflux for 2 hours
3. customAfter the completion of the reaction
4. customprecipitates
5. filtrationwere filtered
6. washThe precipitates were washed with acetonitrile
7. customdried under reduced pressure
8. additionThen, about 20 mL of a saturated sodium hydrogencarbonate solution was added
9. customthe mixture was sonicated for 20 minutes
10. customPrecipitates
11. filtrationwere filtered
12. customrecovered from the resulting mixture
13. washsufficiently washed with water
14. customdried under reduced pressure

ORD record

ord-db33e4ea377546bdaa8b2d43550f899b

Source dataset

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09149546B2