Iodine → HCID 178517806, compound

To a solution of 6-chloropyridin-2-ol (3.00 g, 23.2 mmol) and sodium carbonate (4.88 g, 46.4 mmol) in water (60 mL) was added iodine (5.84 g, 23.0 mmol), and the mixture was stirred at room temperature overnight. The resulting solid was collected by filtration, 1N hydrochloric acid was added to the obtained solid, and the mixture was extracted twice with ethyl acetate. The extract was washed with saturated brine, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, and to the obtained residue were added diisopropyl ether and hexane, and the resulting solid was collected by filtration to give the title compound (1.04 g, yield 18%).

1. filtrationThe resulting solid was collected by filtration, 1N hydrochloric acid
2. additionwas added to the obtained solid
3. extractionthe mixture was extracted twice with ethyl acetate
4. washThe extract was washed with saturated brine
5. dry with materialdried over anhydrous sodium sulfate
6. customThe solvent was evaporated under reduced pressure
7. additionto the obtained residue were added diisopropyl ether and hexane
8. filtrationthe resulting solid was collected by filtration

ORD record

ord-42be48b88d56455c8822a84ed4f3f790

Source dataset

uspto-grants-2013_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08501804B2