Hydrochloric Acid → 4-iodo-3-methylpyridin-2(1H)-one

12M Hydrochloric acid (13 mL) was added to a solution of 2-fluoro-4-iodo-3-methylpyridine (12.2 g) in DME (15 mL) at room temperature. The mixture was stirred at 100 C for 1.5 hours with an alkali trap. Water (150 mL) was added to the reaction mixture at room temperature. The mixture was stirred at the same temperature for 2 hours. The precipitate was collected by filtration, washed with water. A suspension of the solid in ethanol (20 mL) was stirred at 80 C for 30 minutes. Diisopropyl ether (150 mL) was added to the mixture. The mixture was stirred at room temperature for 30 minutes. The precipitate was collected by filtration, washed with diisopropyl ether to give the title compound (9.82 g).

1. stirringThe mixture was stirred at the same temperature for 2 hours
2. filtrationThe precipitate was collected by filtration
3. washwashed with water
4. additionA suspension of the solid in ethanol (20 mL)
5. stirringwas stirred at 80 C for 30 minutes
6. additionDiisopropyl ether (150 mL) was added to the mixture
7. stirringThe mixture was stirred at room temperature for 30 minutes
8. filtrationThe precipitate was collected by filtration
9. washwashed with diisopropyl ether

ORD record

ord-bdc5f5dc5c5e495d8c4e6da4f78a3302

Source dataset

uspto-grants-2015_09

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US09120777B2