反应详情

A mixture of 0.7 g (2.1 mmol) (3,4-Dimethoxy-phenyl)-[2-(4-trifluoromethyl-phenyl)-ethyl]-amine, 0.58 g (2.1 mmol) 2-phenyl-malonic acid monobenzylester (commercially available), 0.83 g (2.5 mmol) TBTU and 0.43 g (4.3 mmol) NEt3 in 15 mL DMF was stirred at room temperature for 16 h. After evaporation to dryness the residue was treated with HCl aq. and DCM. The combined organic phases were washed with HCl aq., dried with MgSO4 and evaporated to dryness. The residue was purified by flash column chromatography on silica eluting with a gradient formed from ethyl acetate and heptane. The product containing fractions were combined and evaporated to dryness to yield 0.35 g (29%) of the title compound. MS(m/e): 578.3 (MH+).

1. customAfter evaporation to dryness the residue
2. additionwas treated with HCl aq. and DCM
3. washThe combined organic phases were washed with HCl aq.
4. dry with materialdried with MgSO4
5. customevaporated to dryness
6. customThe residue was purified by flash column chromatography on silica eluting with a gradient
7. customformed from ethyl acetate and heptane
8. additionThe product containing fractions
9. customevaporated to dryness