反应详情

According to Scheme 1 Step 4: A solution of a mixture of 3-(1-(4-methoxybenzyl)-3-propyl-1H-pyrazol-4-yl)-N-(pyridin-2-yl)-1,2,4-thiadiazol-5-amine and of 3-(1-(4-methoxybenzyl)-5-propyl-1H-pyrazol-4-yl)-N-(pyridin-2-yl)-1,2,4-thiadiazol-5-amine (0.39 mmol, 160 mg) in TFA (2 mL) and dichloroethane (2 mL) was stirred under reflux for 12 hours. After evaporation of the solvent, DCM was added and the organic phase was washed with a saturated solution of NH4OH and brine. Then the organic phase was dried over Na2SO4, was filtered and was concentrated under reduced pressure. The resulting crude product was purified by flash chromatography over silica gel using DCM/MeOH (95:5) as eluent to yield 3-(3-propyl-1H-pyrazol-4-yl)-N-(pyridin-2-yl)-1,2,4-thiadiazol-5-amine (0.24 mmol, 70 mg, 62%) as a white solid.

1. temperatureunder reflux for 12 hours
2. customAfter evaporation of the solvent, DCM
3. additionwas added
4. washthe organic phase was washed with a saturated solution of NH4OH and brine
5. dry with materialThen the organic phase was dried over Na2SO4
6. filtrationwas filtered
7. concentrationwas concentrated under reduced pressure
8. customThe resulting crude product was purified by flash chromatography over silica gel