Methyl iodide → HCID 59635789, compound

NaH (60% in mineral oil, 57 mg) was added to a solution of 4-bromo-1-(3-hydroxy-2-methyl-propyl)-1H-pyridin-2-one (0.53 g) in dimethylformamide (6 mL) chilled in an ice bath. After stirring the solution with cooling for 0.5 h, methyl iodide (110 μL) was added. The cooling bath was removed and the solution was stirred at room temperature overnight. Then, the solution was concentrated under reduced pressure and the residue was diluted with water. The resulting mixture was extracted with ethyl acetate and the combined organic extracts were washed with brine and dried (MgSO4). The solvent was evaporated and the residue was purified by HPLC on reversed phase (acetonitrile/water) to give the title compound as an oil.

1. temperaturechilled in an ice bath
2. temperaturewith cooling for 0.5 h
3. customThe cooling bath was removed
4. stirringthe solution was stirred at room temperature overnight
5. concentrationThen, the solution was concentrated under reduced pressure
6. additionthe residue was diluted with water
7. extractionThe resulting mixture was extracted with ethyl acetate
8. washthe combined organic extracts were washed with brine
9. dry with materialdried (MgSO4)
10. customThe solvent was evaporated
11. customthe residue was purified by HPLC on reversed phase (acetonitrile/water)

ORD record

ord-d15bbd64454c45408229869bae746f50

Source dataset

uspto-grants-2014_01

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08637505B2