Yield:28056-05-5 88%

Reaction Conditions:

with thionyl chloride for 3 h;Reflux;

Steps:

61.1

2-Amino-6-chloroisonicotinic acid (500 mg,2.90 mmol) was dissolved in ethanol (29.0 mL), and the solution was stirred under heat and reflux for 3 hours after adding thionyl chloride (1.06 mL, 14.5 mmol). The solvent was then evaporated under reduced pressure. The residue was extracted with chloroform after adding a sodium hydrogen carbonate aqueous solution. The organic layer was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure to give ethyl 2-amino-6-chloroisonicotinate (510 mg, yield 88%). ¹H NMR (400 MHz, CDCl₃, δ): 7.18 (d, J= 1.0 Hz, 1H), 6.96 (d, J = 1.0 Hz, 1H), 4.70 (s, 2H), 4.37 (q, J= 7.2 Hz, 2H), 1.39 (t, J = 7.1 Hz, 3H)

References:

EP2671582,2013,A1 Location in patent:Paragraph 0552