2-Aminonicotinic acid → Methyl 2-aminopyridine-3-carboxylate

Temperature

90 °C

The mixture of 138 mg of 2-aminonicotinic acid and 6 mL of hydrochloric acid-methanol solution was stirred overnight in a sealed-tube at 90° C. The reaction mixture was concentrated under reduced pressure, the residue was added with a saturated aqueous solution of sodium hydrogen carbonate, and extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, the insolubles were filtered, and the filtrate was concentrated under reduced pressure, to obtain 106 mg of 2-aminonicotinic acid methylester [25-1]. The obtained compound [25-1] was used in the subsequent reaction without further purification.

1. concentrationThe reaction mixture was concentrated under reduced pressure
2. additionthe residue was added with a saturated aqueous solution of sodium hydrogen carbonate
3. extractionextracted with ethyl acetate
4. dry with materialThe organic layer was dried over anhydrous sodium sulfate
5. filtrationthe insolubles were filtered
6. concentrationthe filtrate was concentrated under reduced pressure

ORD record

ord-0daa06293d5f44b9b7ca85a76e2a2e9e

Source dataset

uspto-grants-2010_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07718801B2