Citric Acid → HCID 71178972, compound

Participants

Reaction Conditions

Reaction Steps

2,2-Difluorocyclopropanecarboxylic acid (0.067 g, 0.552 mmol) was dissolved in 1,4-dioxane (2 mL), diphenylphosphoryl azide (0.182 g, 0.66 mmol) and triethylamine (0.092 mL, 0.66 mmol) were added, and the mixture was heated under reflux for 2 hr. The reaction solution was allowed to cool, 7-(2-chloro-5-methylphenylamino)-6-[4-(4-fluorophenyl)piperidine-1-carbonyl]pyrazolo[1,5-a]pyrimidine-3-sulfonamide (0.10 g, 0.18 mmol) obtained in Example 12 step 5 and potassium carbonate were added, and the mixture was stirred at 50° C. for 3 hr. 5% Aqueous citric acid solution was added to quench the reaction, and the precipitated crystals were collected by filtration. The obtained crystals were purified by silica gel column chromatography (chloroform/methanol=10/1) to give the title compound (0.014 g, 11%).

Provenance & Evidence