1-Methylpiperazine → 1-[4-(2,5-Dichlorophenoxy)-4-(2-thienyl)butyl]-4-methyl-piperazine difumarate

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Reaction Steps

The product from Example 19 step (c) (0.35 g, 0.83 mmol) was dissolved in anhydrous tetrahydrofuran (10 ml) and N-methylpiperazine (0.25 g, 2.49 mmol) added and stirred at room temperature for, 18 h. The precipitated white solid was filtered off and discarded. The filtrate was evaporated and the residue dissolved in methanol and placed on a CC SCX resin. After washing with methanol (150 ml), the product was liberated with 7N ammonia in methanol (100 ml). The solvents were evaporated and the residue dissolved in methanol, treated with one equivalent of fumaric acid, and stirred for ten minutes. The solvent was removed in vacuo and the solid residue recrystallised from hot isopropanol to afford the title compound (0.13 g, 30%).

Provenance & Evidence