Triethylamine → HCID 117840283, compound

Participants

Reaction Steps

To a solution of (3R)-3-ethyl-2-oxo-1-(2-((4-(piperazin-1-yl)phenyl)amino)pyrimidin-4-yl)pyrrolidine-3-carbonitrile (100 mg) obtained in Example 220 in tetrahydrofuran (3.0 mL) were added successively dropwise triethylamine (71 μL) and methanesulfonyl chloride (24 μL) in an ice bath, and the mixture was stirred at the same temperature for 3 hr. To the reaction mixture was added saturated aqueous ammonium chloride solution, and the solvent was evaporated under reduced pressure. The residue was purified by silica gel column chromatography (hexane/ethyl acetate), to a solution of the obtained purified product (120 mg) in ethanol (3 mL) was added 1 M hydrochloric acid (0.25 mL), and the mixture was stirred at room temperature for 5 min. The solvent was evaporated under reduced pressure, and the residue was recrystallized (ethanol/diisopropyl ether) to give the title compound (91 mg).

Provenance & Evidence