反应详情

温度

60 °C

0.5 g of 2-tert-Butyl-4-[4-(3-chloro-propyl)-piperazin-1-yl]-6-cyclobutyl-pyrimidine (1.42 mmol) were dissolved in 15 ml of dimethylformamide. 0.18 g of 1-methyl-1H-tetrazole-5-thiol (1.56 mmol), 0.09 g of lithium hydroxide (3.76 mmol) and a spatula tip of potassium iodide were added. The mixture was stirred for 2 h at 60° C. After cooling to room temperature, the reaction mixture was partitioned between water and ethyl acetate. The ethyl acetate layer was dried over magnesium sulfate, filtered, and the solvent evaporated under vacuum. The resulting crude product was purified by column chromatography on silica gel using dichloromethane-methanol (1-5%). Fractions containing the product were combined and the solvent was evaporated under vacuum. The residue was treated with acetonitril, the solvent evaporated, whereby 0.3 g of the title compound were obtained as an oily residue.

1. temperatureAfter cooling to room temperature
2. customthe reaction mixture was partitioned between water and ethyl acetate
3. dry with materialThe ethyl acetate layer was dried over magnesium sulfate
4. filtrationfiltered
5. customthe solvent evaporated under vacuum
6. customThe resulting crude product was purified by column chromatography on silica gel
7. additionFractions containing the product
8. customthe solvent was evaporated under vacuum
9. additionThe residue was treated with acetonitril
10. customthe solvent evaporated