Sodium Hydroxide → HCID 178517757, compound

To a solution of NaOH (101 g, 2.5 mol) in water (500 mL) was added 5-chloro-2,3-difluoropyridine (101 g, 0.68 mol) as a liquid, and the resulting mixture was heated to reflux overnight. After cooling to room temperature, the mixture was filtered through a pad of celite and the pH was adjusted to 1 by the addition of concentrated HCl. The resulting solid was removed by filtration and dissolved in ethyl acetate. The combined organic layers were dried over sodium sulfate, filtered and concentrated in vacuo. The title compound was obtained as a white solid (78 g, 78%) and was used without additional purification. The product was characterized by 1H NMR.

1. temperaturethe resulting mixture was heated
2. temperatureto reflux overnight
3. filtrationthe mixture was filtered through a pad of celite
4. additionthe pH was adjusted to 1 by the addition of concentrated HCl
5. customThe resulting solid was removed by filtration
6. dissolutiondissolved in ethyl acetate
7. dry with materialThe combined organic layers were dried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo

ORD record

ord-47e1bd30768240caa58ea6102ac20660

Source dataset

uspto-grants-2010_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07851484B2