反应详情

4-Methyl-5-quinolin-6-yl-4H-[1,2,4]triazole-3-thiol (0.5 g, 2.07 mmol), 2-(3-Bromo-propyl)-5,5-dimethyl-[1,3]dioxane (0.49 g, 2.07 mmol) and lithium hydroxide (50 mg) were heated in dimethylformamide at 100° C. for 3 h. The mixture was cooled and partitioned between water (80 ml) and ethyl acetate (100 ml). The layers were separated and the aqueous re-extracted with ethyl acetate (100 ml). The combined organic portions were washed with brine (100 ml) and then dried (Na2SO4), filtered and evaporated to give a colourless oil. Purification by silica gel chromatography (eluent EtOAc—10% MeOH:EtOAc) which gave the title compound as a colourless solid (0.53 g, 65%).

1. temperatureThe mixture was cooled
2. custompartitioned between water (80 ml) and ethyl acetate (100 ml)
3. customThe layers were separated
4. extractionthe aqueous re-extracted with ethyl acetate (100 ml)
5. washThe combined organic portions were washed with brine (100 ml)
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. customevaporated
9. customto give a colourless oil
10. customPurification by silica gel chromatography (eluent EtOAc—10% MeOH:EtOAc) which