3,5-Difluoropyridine-2-carboxylic acid → 3,5-difluoro-N-methylpyridine-2-carboxamide

温度

50 °C

N,N′-carbonyldiimidazole (600 mg) was added to a solution of 3,5-difluoropyridine-2-carboxylic acid (500 mg) in THF (10 ml), followed by stirring at 50° C. for one hour. The reaction solution was returned to room temperature, a 40% methylamine/methanol solution (1 ml) was added thereto, followed by stirring at room temperature for one hour. The reaction solution was concentrated and the residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 0:100 linear gradient) to obtain 3,5-difluoro-N-methylpyridine-2-carboxamide (293 mg) as a colorless solid.

1. customwas returned to room temperature
2. stirringby stirring at room temperature for one hour
3. concentrationThe reaction solution was concentrated
4. customthe residue was purified by silica gel column chromatography (hexane:ethyl acetate=100:0 to 0:100 linear gradient)

ORDレコード

ord-542ff3a5fff6400e99c84b91f9847ebe

出典データセット

uspto-grants-2013_02

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08377923B2