Sulfuric Acid → HCID 19968428, compound

Participants

Reaction Steps

5-(4-Fluorophenyl)-5-hydroxy-1-azaspiro[5.5]undecane (1.27 g, prepared in a similar manner to that described in Example F) was dissolved in concentrated sulphuric acid (25 ml) and stirred at ambient temperature for 2 hours, then the solution was carefully poured onto ice (50 ml), and the sticky solid collected by filtration. The solid was triturated with ether (2×50 ml), collected by filtration, washed with ether and dried in vacuo at ambient temperature to give a solid which was triturated with hot ether (70 ml), collected by filtration washed with ether and dried in vacuo at 60° C. to give 5-(4-fluorophenyl)-1-azaspiro[5.5]undec-4-ene sulphate as a white solid. Yield 1.3 g, mp 195°-200° C.

Provenance & Evidence