反应详情

To a suspension of 7 g of 3-tosyloxymethyl-4-(3-o-chlorobenzoyl-5-ethyl-2-thienyl)-5-methyl-4H-1,2,4-triazole in 100 ml of ethanol is added 2 g of N-methyl-piperazine, and the mixture is refluxed for 5 hours. Aftr the completion of the reaction, the solvent is distilled off and water is added to the residue. The residue is made alkaline with potassium carbonate and extracted with ethyl acetate. The extract is washed with water and dried over anhydrous sodium sulfate. The solvent is distilled off and the residue obtained is allowed to react with 2.2 g of oxalic acid in ethanol. The crude crystals formed are recrystallized from aqueous ethanol to give 3.8 g of 3-(4-methyl-1-piperazinylmethyl)-4-(3-o-chlorobenzoyl-5-ethyl-2-thienyl)-5-methyl-4H-1,2,4-triazole dioxalate 1/2 hydrate as colorless crystals melting at 164° - 165°C (decomposition).

1. temperaturethe mixture is refluxed for 5 hours
2. customAftr the completion of the reaction
3. distillationthe solvent is distilled off
4. additionwater is added to the residue
5. extractionextracted with ethyl acetate
6. washThe extract is washed with water
7. dry with materialdried over anhydrous sodium sulfate
8. distillationThe solvent is distilled off
9. customthe residue obtained
10. customThe crude crystals formed
11. customare recrystallized from aqueous ethanol