反应详情

A mixture of 4′-({4-[trans-4-(2-hydroxyethoxy)cyclohexyl]-5-oxo-7-propyl-4,5-dihydro[1,2,4]triazolo[1,5-a]pyrimidin-6-yl}methyl)biphenyl-2-carbonitrile (0.2 g), p-toluenesulfonyl chloride (0.089 g), triethylamine (0.066 mL), 4-dimethylaminopyridine (0.005 g) and acetonitrile (10 mL) was stirred for 4 hr. The reaction mixture was washed with water and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was dissolved in acetonitrile (15 mL), sodium thiomethylate (15% aqueous solution, 1.8 g) was added, and the mixture was stirred at 50° C. for 16 hr. The reaction mixture was diluted with ethyl acetate, washed with water and then with saturated brine, and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure. The obtained residue was purified by silica gel column chromatography to give the title compound as a colorless solid (0.2 g, 94%).

1. washThe reaction mixture was washed with water
2. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
3. customThe solvent was evaporated under reduced pressure
4. dissolutionThe obtained residue was dissolved in acetonitrile (15 mL)
5. additionsodium thiomethylate (15% aqueous solution, 1.8 g) was added
6. stirringthe mixture was stirred at 50° C. for 16 hr
7. additionThe reaction mixture was diluted with ethyl acetate
8. washwashed with water
9. dry with materialwith saturated brine, and dried over anhydrous magnesium sulfate
10. customThe solvent was evaporated under reduced pressure
11. customThe obtained residue was purified by silica gel column chromatography