2-Aminonicotinic acid → 3-Pyridinecarboxylic acid, 2-amino-, 2-[4-(1-methylethyl)benzoyl]hydrazide

A mixture of 4-(1-methylethyl)benzohydrazide (2194 mg), HOBt.H2O (2073 mg), EDCI HCl (2595 mg) and 2-aminopyridine-3-carboxylic acid (1700 mg) in dehydrated DMF (50 mL) was stirred at 60° C. overnight. The reaction mixture was added to a saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine, dried over anhydrous magnesium sulfate and concentrated under reduced pressure. The residue was crystallized from a mixture of ethyl acetate and diisopropyl ether to give the title compound (2.4489 g) as a white solid. The mother liquor was purified by silica gel column chromatography (ethyl acetate/hexane) to give the title compound (276.1 mg) as a white solid.

1. extractionthe mixture was extracted with ethyl acetate
2. washThe organic layer was washed with saturated aqueous sodium hydrogen carbonate solution and saturated brine
3. dry with materialdried over anhydrous magnesium sulfate
4. concentrationconcentrated under reduced pressure
5. customThe residue was crystallized from a mixture of ethyl acetate and diisopropyl ether

ORD 기록

ord-c7cadd9ea65d4b409e9bb7868ca11c23

출처 데이터셋

uspto-grants-2013_11

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US08575154B2