Ethanol → 5-Bromo-3-methylpyridine-2-carboxylic acid

Temperatur

80 °C

To a solution of 5-bromo-3-methylpyridine-2-carbonitrile (3.9 g, 20 mmol) in ethanol (30 mL) was added 6.0 M sodium hydroxide in water (15 mL), and the reaction was stirred at 80° C. for 1.5 h. The reaction mixture was concentrated, diluted with water and partitioned in EtOAc. The aqueous phase was acidified to pH 2-3. The product then was extracted with EtOAc, washed with brine, dried over sodium sulfate, filtered and concentrated to give 4.2 g (98% yield) of the desired product as a yellow solid.

1. concentrationThe reaction mixture was concentrated
2. additiondiluted with water
3. custompartitioned in EtOAc
4. extractionThe product then was extracted with EtOAc
5. washwashed with brine
6. dry with materialdried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated

ORD-Eintrag

ord-42d5aabd18344f79b54970cdd1038d4b

Quelldatensatz

uspto-grants-2014_11

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08895571B2