2-Pyridinamine, 5-iodo- → HCID 77985005, compound

Temperature

100 °C

657 mg (corresponding to 2.46 mmol) of 5-(2-bromoacetyl)-2-(1H-1,2,4-triazole-1-yl)pyridine and 541 mg (corresponding to 2.46 mmol) of 2-amino-5-iodopyridine were dissolved in 5.0 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 10 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 675 mg (corresponding to 1.74 mmol) of 6-iodo-2-[2-(1H-1,2,4-triazole-1-yl)pyridine-5-yl]imidazo[1,2-a]pyridine (FIG. 4, 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 10 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-4035f551d69e4e7ba8aa75827ec4773b

Source dataset

uspto-grants-2015_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09211350B2