Triethylamine → 3-[2-(4-(3-Trifluoromethylphenyl)piperazin-1-yl)ethylmercapto]-8-trifluoromethyl-1,2,4-triazolo(4,3-a)pyridine maleate

関与物質

反応手順

A solution of 11 g of 3-mercapto-8-trifluoromethyl-1,2,4-triazolo(4,3-a)pyridine, prepared in Example 18, and 15 g of 1-chloro-2-[4-(3-trifluoromethylphenyl)piperazin-1-yl]ethane in 75 ml of ethanol containing 8 ml of triethylamine is heated under reflux for 6 hours. The reaction mixture is then concentrated in vacuo, water and ice are added and the extraction is carried out with ether. The organic phase is washed with water, with a dilute solution of sodium hydroxide and then again with water. The ether phase is dried and then concentrated and the residue obtained (21.5 g) is dissolved in acetone. A solution of 5.1 g of maleic acid in acetone is added to this acetone solution. The crystals which then form are filtered off, washed with acetone and ether and dried to give 11.5 g of 3-[2-(4-(3-trifluoromethylphenyl)piperazin-1-yl)ethylmercapto]-8-trifluoromethyl-1,2,4-triazolo(4,3-a)pyridine maleate in the form of crystals melting at 144°-5° C.

情報源と証拠