Potassium hydroxy sulfite → HCID 53236491, compound

Participants

Reaction Conditions

Reaction Steps

A 6 mL aliquot of 2-pyrazol-1-yl-5-trifluoromethyl-benzaldehyde from the above reaction is filtered (in DMF, 50% pure by LC-MS, calculated mass based on purity is 98 mg, 0.41 mmol). The crude aldehyde is treated with 4-(2-amino-pyrimidin-5-yl)-N1-tert-butyl-benzene-1,2-diamine (100 mg, 0.39 mmol). Oxone (239 mg, 0.39 mmol) is added as a water solution (1 mL). The resulting mixture is warmed to 60° C. for 2 hours and cooled to room temperature, poured into water and extracted with EtOAc (3×). The combined organics are dried (MgSO4), filtered, and concentrated. Purification via flash chromatography (12 g silica gel, 0-6% MeOH/CH2Cl2) follows by mass triggered HPLC (CH3CN/H2O) affords the title compound (40 mg, 22%). LCMS (ESMS): m/z 478.20 (M++1)

Provenance & Evidence