Acetonitrile → Dasatinib monohydrate

Participants

Reaction Conditions

Reaction Steps

200 ml of acetonitrile was taken in RB flask and 10.0 g of 2-((6-chloro-2-methylpyrimidin-4-yl)amino)-N-(2-chloro-6-methylphenyl)thiazole-5-carboxamide (Formula I), 19.8 g of 1-(2-Hydroxyethyl)piperazine (Formula II), 12.85 g of triethyl amine and 10.0 g of TBAB were charged into it. The reaction mass was stirred for 10-15 mins at 30-35° C. and then heated to 80° C. and stirred for 20-22 h. The completion of reaction was checked with Thin Layer Chromatography (TLC) and 300 mL of water was slowly charged. The reaction mass was stirred for 45 mins at 80° C. and then cooled to 30-35° C. and further stirred for ˜1.5 hrs. The reaction mass was filtered, washed with 20 mL water and suck dried for 10-15 min at RT. The wet compound was unloaded and air dried for 30 mins at 30-35° C. The material was loaded to a vacuum tray drier at 30-35° C. and vacuum was applied. The material was dried at 30-35° C. for 1 h and slowly dryer temperature was raised to 50-55° C. where drying was carried out for 8-10 hrs. The solid product obtained was then cooled to 30-35° C. and vacuum was released to obtain 12.5 g of the title compound.

Provenance & Evidence