反应详情

Pyridazine-3-carboxylic acid (CAN 2164-61-6; 43.1 mg, 347 μmol) was suspended in DMF (1.0 mL). TBTU (112 mg, 347 μmol), ethyldiisopropylamine (102 mg, 131 μl, 789 μmol,) and 5-(4-chloro-phenyl)-6-((S)-2,2,2-trifluoro-1-methyl-ethoxy)-pyridin-3-ylamine (0.100 g, 316 μmol) were added and the reaction mixture was stirred at room temperature for 1 h. The rection mixture was extracted with ethyl acetate and 1M citric acid solution; the organic phase was dried with MgSO4 and concentrated in vacuo. The crude material was purified by flash chromatography (silica gel, 10 g, 10% to 50% ethyl acetate in heptane) to give 0.11 g (83%) of the title compound as white solid; MS (EI) 423.1 (M+H)+.

1. extractionThe rection mixture was extracted with ethyl acetate and 1M citric acid solution
2. dry with materialthe organic phase was dried with MgSO4
3. concentrationconcentrated in vacuo
4. customThe crude material was purified by flash chromatography (silica gel, 10 g, 10% to 50% ethyl acetate in heptane)