5-chloro-N3-ethylpyridazine-3,4-diamine synthesis

Yield:1614246-24-0 51%

Reaction Conditions:

at 120; for 48 h;Sealed tube;

Steps:

7 5-Chloro-N3-ethylpyridazine-3,4-diamine

A mixture of 3,5-(dichloropyridazin-4-yl)amine (Preparation 4, 15 g, 92 mmol) and anhydrous ethylamine (50 mE) was heated to 120° C. for 48 hours in a sealed tube. The reaction mixture was cooled to room temperature, and then added to a mixture of water (500 mE) and EtOAc (50 mL). The resulting precipitate was separated by filtration and the filter cake was washed with tEME, and dried under vacuum to afford the title compound as off-white solid in 51% yield, 8.1g.10464] ‘H-NMR (400 MHz, DMSO-d5): ? ppm 1.18 (t,3H), 3.41 (q, 2H), 6.08-6.11 (m, 3H), 8.09 (s, 1H).

References:

US2014/171435,2014,A1 Location in patent:Paragraph 0463; 0464