3-FluoropicoliniMidaMide hydrochloride synthesis

Yield:246872-67-3 1.15 g

Reaction Conditions:

with diisobutylaluminum hydride;ammonium chloride in toluene at 80;

Steps:

145.A A) 3-fluoropicolinimidamide hydrochloride

To a mixture of ammonium chloride (1.34 g) and toluene (15 mL) was added a solution (1.5 M, 15.3 mL) of diisobutylaluminum hydride in toluene at 0°C, and the mixture was stirred at 80°C for 20 min.
To the reaction mixture was added 3-fluoropyridine-2-carbonitrile (0.6 g), and the mixture was stirred at 80°C overnight.
To the reaction mixture was added methanol at 0°C, and the mixture was stirred at room temperature for 3 hr, filtered, and insoluble material was washed with methanol.
The obtained filtrate was concentrated under reduced pressure, and the residue was washed with ethyl acetate to give the title compound (1.15 g).
MS: [M+H]⁺ 140.1.

References:

EP3061754,2016,A1 Location in patent:Paragraph 0623