1-(6-chloropyrimidin-4-yl)-3-methyl-1H-pyrazol-5-amine synthesis

Yield:-

Reaction Conditions:

in isopropyl alcohol at 85; for 5 h;

Steps:

5

The mixture of (6-chloro-pyrimidin-4-yl)-hydrazine (16.97 g, 117 mmol),3-imino-butyronitrile (28.88 g, 352 mmol), and 2-propanol (500 mL) was heated to 85°C for 5 h. The reaction mixture was then cooled to room temperature, condensed, and recrystallized from ethanol/water (1 : 1, 400 mL). The solid was filtered and washed with water (200 mL), then ethanol/water (1 : 1, 100 mL), dried to afford the desired product 20 .66 g. An additional product (0.9 g) was isolated from the filtrate after standing overnight at room temperature. MS m/z 210.05 (M + 1).

References:

WO2008/42639,2008,A1 Location in patent:Page/Page column 81