Formic Acid → HCID 86593203, compound

Temperature

50 °C

To acetic anhydride (2.39 ml) was added dropwise formic acid (0.97 ml) under ice-cooling, and the mixture was stirred at 50° C. for 30 minutes. The mixture was ice-cooled again, and diluted with tetrahydrofuran (9 ml). To the mixture were added 2-amino-1-(3-pyridyl)-1-butanone dihydrochloride (600 mg) and triethylamine (1.41 ml), and the mixture was stirred under ice-cooling for 1.5 hours. To the reaction mixture was added a saturated aqueous sodium hydrogen carbonate solution, and the mixture was extracted with ethyl acetate. The organic layer was washed with brine, dried over anhydrous sodium sulfate and the solvent was removed under reduced pressure. The resulting residue was triturated with ethyl acetate-diethyl ether to obtain 2-formylamino-1-(3-pyridyl)-1-butanone (440 mg) as colorless powder.

1. temperaturecooling
2. temperaturecooled again
3. stirringthe mixture was stirred under ice-
4. temperaturecooling for 1.5 hours
5. extractionthe mixture was extracted with ethyl acetate
6. washThe organic layer was washed with brine
7. dry with materialdried over anhydrous sodium sulfate
8. customthe solvent was removed under reduced pressure
9. customThe resulting residue was triturated with ethyl acetate-diethyl ether

ORD record

ord-ab6077cd3c624db296ad87e0ee0d9856

Source dataset

uspto-grants-2010_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07759373B2