Bromine → HCID 178517592, Verbindung

A solution of 2-hydroxy-3-(trifluoromethyl)pyridine (10.0 g) and bromine (3.08 ml, 9.60 g) in methanol (50 ml) was stirred at 20° C. for 22 h. The solution was concentrated and the residue partitioned between ethyl acetate (400 ml) and water (100 ml). The layers were separated and the organic layer was washed with 5% Na2S2O3aq. (100 ml) and brine (100 ml), dried over sodium sulphate, filtered and concentrated. Purified by Biotage SNAP cartridge KP-Sil column twice (100 g, heptane:ethyl acetate=1:0, 3:1 to 2:1) to give 13.69 g light yellow solid as 5-bromo-2-hydroxy-3-(trifluoromethyl)pyridine (95%).

1. concentrationThe solution was concentrated
2. customthe residue partitioned between ethyl acetate (400 ml) and water (100 ml)
3. customThe layers were separated
4. washthe organic layer was washed with 5% Na2S2O3aq
5. dry with material(100 ml) and brine (100 ml), dried over sodium sulphate
6. filtrationfiltered
7. concentrationconcentrated
8. customPurified by Biotage SNAP cartridge KP-Sil column twice (100 g, heptane:ethyl acetate=1:0, 3:1 to 2:1)

ORD-Eintrag

ord-a9b9b295723d4dd89022c3f180cfbf97

Quelldatensatz

uspto-grants-2015_08

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09115126B2