2-Pyridinamine, 5-iodo- → HCID 77985002, compound

Temperature

100 °C

66.4 mg (corresponding to 0.249 mmol) of 5-(2-bromoacetyl)-2-(1H-1,2,3-triazole-1-yl)pyridine and 54.8 mg (corresponding to 0.249 mmol) of 2-amino-5-iodopyridine were dissolved in 2.0 mL of acetonitrile. The resulting solution was heated under reflux for 1.5 hours in an oil bath at 100° C. 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 2 mL of water and 2 mL of methanol. Then, about 1 mL of a saturated sodium hydrogencarbonate solution was added thereto, and the mixture was 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 44.0 mg (corresponding to 0.113 mmol) of 6-iodo-2-[2-(1H-1,2,3-triazole-1-yl)pyridine-5-yl]imidazo[1,2-a]pyridine (FIG. 1, step 3).

1. temperatureThe resulting solution was heated
2. customAfter the completion of the reaction
3. temperaturethe reaction solution was cooled down to room temperature
4. customprecipitates
5. filtrationwere filtered
6. washThe precipitates were washed with acetonitrile
7. customdried under reduced pressure
8. additionThen, about 1 mL of a saturated sodium hydrogencarbonate solution was added
9. customthe mixture was sonicated for 5 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-0eef44730ecd48139d83064850fc35ab

Source dataset

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09211350B2