反应详情

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.

1. temperatureis heated
2. temperatureunder reflux for 6 hours
3. concentrationThe reaction mixture is then concentrated in vacuo, water and ice
4. additionare added
5. extractionthe extraction
6. washThe organic phase is washed with water, with a dilute solution of sodium hydroxide
7. dry with materialThe ether phase is dried
8. concentrationconcentrated
9. customthe residue obtained (21.5 g)
10. customThe crystals which then form
11. filtrationare filtered off
12. washwashed with acetone and ether
13. customdried