Sodium hydride → HCID 178432162, compound

To a mixture of 3-mercapto-1H-1,2,4-triazole (1.15 g) and N,N-dimethylformamide (15 ml) was added 60% sodium hydride (450 mg). After foaming was completed, N-chlorosuccinimide in small portions was added to the mixture on an ice bath, and stirred at this temperature for 15 minutes. 2-methylimidazo[1,2-a]pyridine (1.0 g) was then added, and the reaction mixture was heated and stirred at room temperature for 1 hour, and then for 3 hours on an oil bath at 70° C. The reaction solution was concentrated under reduced pressure. The residue was washed twice with diethyl ether, and methanol was added to the residue to remove undissolved materials. The filtrate was concentrated, and then crystals precipitated by the addition of water were collected by filtration, washed with water, followed by diethyl ether, and dried to yield the title compound (480 mg).

1. temperaturethe reaction mixture was heated
2. stirringstirred at room temperature for 1 hour
3. waitfor 3 hours on an oil bath at 70° C
4. concentrationThe reaction solution was concentrated under reduced pressure
5. washThe residue was washed twice with diethyl ether, and methanol
6. additionwas added to the residue
7. customto remove undissolved materials
8. concentrationThe filtrate was concentrated
9. customcrystals precipitated by the addition of water
10. filtrationwere collected by filtration
11. washwashed with water
12. customdried

ORD record

ord-3b7f962087a64baf933ae68db9e574c6

Source dataset

uspto-grants-2007_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07238720B2