N~1~-(5-amino-2-methylphenyl)-N~2~,N~2~-dimethylglycinamide(SALTDATA: FREE) synthesis

Yield:946753-98-6 72.4%

Reaction Conditions:

with hydrogenchloride in 1,4-dioxane at 25; for 2 h;

Steps:

24.B

To a solution of tert-butyl 3-(2-(dimethylamino)acetamido)-4-methylphenylcarbamate (0.615 g, 2 mmol) in 1,4-dioxane (2 mL) was added 4N HCl in 1,4-dioxane (2 mL). The solution was stirred at 25°C for 2 hours. Filtration provided the title compound as a white solid (0.30 g, 1.447 mmol, 72.4% yield); ¹H NMR (400 MHz, DMSO-d₆) δ 10.44 (s, 2H), 10.18 (br. s., 3H), 7.56 (d, J = 2.34 Hz, IH), 7.36 (d, J = 8.20 Hz, IH), 7.16 (dd, J = 2.15, 8.00 Hz, IH), 4.26 (S₅ 2H), 2.88 (s, 6H), 2.26 (s, 3H).

References:

WO2009/89042,2009,A1 Location in patent:Page/Page column 120-121