反应详情

A mixture of 16 g of 4,4-bis(p-fluorophenyl)cyclohexyl mesylate, 10 g of 1-(p-fluorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one (m.p. 234°-234.5° C), 6.1 g of potassium carbonate, 7.3 g of potassium iodide and 100 ml of dimethylformamide is stirred at 70°-80° C for 50 hours. The reaction mixture is poured into water, isopropyl ether is added to the aqueous mixture, and the resulting mixture is stirred for some time. The precipitated crystals are collected by filtration and dissolved in a mixture of chloroform and methanol (9:1). The solvent is removed to some degree and cooled in an ice bath. The precipitated crystals are collected by filtration and purified in the same manner to give 8-[4,4-bis(p-fluorophenyl)cyclohexyl]-1-(p-fluorophenyl)-1,3,8-triazaspiro[4.5]decan-4-one as white crystals, melting at 237°-240° C.

1. additionis added to the aqueous mixture
2. stirringthe resulting mixture is stirred for some time
3. filtrationThe precipitated crystals are collected by filtration
4. dissolutiondissolved in a mixture of chloroform and methanol (9:1)
5. customThe solvent is removed to some degree
6. temperaturecooled in an ice bath
7. filtrationThe precipitated crystals are collected by filtration
8. custompurified in the same manner