Acetonitrile → Dasatinib monohydrate

Participants

Reaction Conditions

Reaction Steps

Take 12 ml of acetonitrile in RB flask and charge 1 g of 2-((6-chloro-2-methylpyrimidin-4-yl)amino)-N-(2-chloro-6-methylphenyl)thiazole-5-carboxamide (Formula I), 1.98 g of 1-(2-Hydroxyethyl)piperazine (Formula II), 1.28 g of triethyl amine and 1.02 g of TBAB. Stir the reaction mass for 10-15 min at 30-35° C. Heat the reaction mixture to 75-80° C. and stir for 20-24 h. Check for the completion of reaction with Thin Layer Chromatography (TLC). Charge 4 mL of water slowly and stir the reaction mass for 30-45 mins at 75° C. Cool the reaction mass to 30-35° C. and stir for 2-3 hrs. Filter the reaction mass and wash with acetonitrile and water mixture (1:1). Dry the material to get 1.15 g of crystalline Dasatinib monohydrate.

Provenance & Evidence