6-chloro-N-cyclopropyl-3-nitropyridin-2-amine synthesis

Yield:380378-95-0 89%

Reaction Conditions:

in water;toluene;

Steps:

III.a a

a 6-Chloro-2-(cyclopropylamino)-3-nitropyridine A solution of cyclopropylamine (1.25 g, 22.0 mmol) in toluene (11 mL) was added over 10 min to an ice-cold solution of 2,6-dichloro-3-nitropyridine (2.00 g, 10.4 mmol) in toluene (10 mL). The mixture was stirred at 0° C. for 1 h and at room temperature for 2 h. Water (50 mL) was added to the mixture and the phases were separated. The organic layer was washed with brine (25 mL), dried (MgSO₄), filtered and concentrated under reduced pressure. The residue was purified by flash chromatography (hexane:EtOAc, 3:2) to give the title compound (1.97 g, 89% yield) as a yellow solid.

References:

US2002/28807,2002,A1