Dichloromethane → HCID 23090364, compound

Participants

Reaction Steps

To a solution of 4-[1-(6-methoxy-3-pyridyl)-5-phenylpyrazole-3-carbonyl]piperazine-1-carboxylic acid tert-butyl ester (332 mg) obtained in Example 64 in methylene chloride (2 mL), anisole (0.4 mL) and trifluoroacetic acid (1.6 mL) were added, and the mixture was stirred at room temperature for 30 minutes. The reaction solvent was removed under reduced pressure, and the residue was partitioned between water and diethyl ether. The aqueous layer was alkalinized with saturated aqueous sodium hydrogencarbonate and extracted with ethyl acetate four times. The organic layers were combined, followed by drying over sodium sulfate anhydrate. After filtration, the solvent was removed under reduced pressure. The residue was dissolved in a solvent mixture of diethyl ether and a small amount of methanol. 1M HCl-ethanol (0.78 mL) was added thereto, and the precipitated crystals were collected through filtration. The thus-obtained matter was recrystallized from methanol-diethyl ether, to thereby give the title compound (229 mg, 76%).

Provenance & Evidence