反应详情

温度

11 °C

Methyl 4-amino-3-phenylbutanoate hydrochloride x11 (0.19 g, 0.83 mmol, 1.05 eq) is added to a solution of aldehyde x235 (0.17 g, 0.79 mmol) in dry dichloroethane (DCE) (7.8 ml). The mixture is kept at room temperature for 30 min, cooled to 10-12° C., and a solution of triethylamine (0.15 ml, 0.83 mmol, 1.05 eq) in dry DME (2.5 ml) is added dropwise. The mixture is additionally stirred at the same temperature for 1 h and cooled to 0-5° C. Then STAB (0.23 g, 1.10 mmol, 1.4 eq) is added in portions under vigorous stirring. The mixture is additionally stirred at 0-5° C. for 30 min and kept at room temperature overnight. Then the mixture is heated to 60° C. for 2 h and cooled to room temperature. An equal volume of dichloromethane is added, and the mixture is washed with 10% K2CO3 (2×10 ml). The mixture is dried over anhydrous Na2SO4 and evaporated. The oily residue is triturated with ether, and the formed crystals are separated by filtration, washed twice with ether, and vacuum-dried to give white fine-crystalline 4-phenyl-1-{[3-(trifluoromethyl)[1,2,4]triazolo[4,3-b]pyridazin-7-yl]methyl}pyrrolidin-2-one 255.

1. temperaturecooled to 0-5° C
2. additionThen STAB (0.23 g, 1.10 mmol, 1.4 eq) is added in portions under vigorous stirring
3. stirringThe mixture is additionally stirred at 0-5° C. for 30 min
4. waitkept at room temperature overnight
5. temperatureThen the mixture is heated to 60° C. for 2 h
6. temperaturecooled to room temperature
7. washthe mixture is washed with 10% K2CO3 (2×10 ml)
8. dry with materialThe mixture is dried over anhydrous Na2SO4
9. customevaporated
10. customThe oily residue is triturated with ether
11. customthe formed crystals are separated by filtration
12. washwashed twice with ether
13. customvacuum-dried