Sodium hydride → 4,5-Dihydro-5-thioxo-8-(3-(trifluoromethyl)phenyl)-3H,6H-1,4,5a,8a-tetraazaacenaphthylene-3-one

Beteiligte Stoffe

Reaktionsbedingungen

Reaktionsschritte

To a stirred solution of 1.00 g of 4,5-dihydro-7-(3-(trifluoromethyl)phenyl)pyrazolo(1,5-a)pyrimidine-3-carboxamide (prepared as described in Example 8) in 30 ml of dry tetrahydrofuran cooled to -78° C. is added 286 mg of 60 percent sodium hydride (dispersion in mineral oil). The reaction mixture is stirred at -78° C. for 30 minutes then 637 mg of 1,1'-thiocarbonyldiimidazole is added and the mixture is allowed to slowly warm to room temperature and then is stirred for 36 hours. The mixture is quenched with water, neutralized with 5 percent aqueous hydrochloric acid and extracted with chloroform. Evaporation of the extract in vacuo gives 934 mg of the desired product.

Herkunft & Nachweise