反应详情

温度

120 °C

A mixture of the above N,N-dimethyl-N′-[3-trifluoromethyl-5-(4-trifluoromethyl-phenyl)-pyridin-2-yl]-formamidine (3.61 g, 10.0 mmol) and ethyl bromoacetate (3.32 mL, 30.0 mmol) in DMF (10 mL) was stirred at 120° C. for 4 h. Cooled down to 100° C., added DIPEA (0.5 mL, 3.0 mmol) and stirred at 23° C. for 2 h. Poured into sat. NaHCO3-sol., extracted with EtOAc, washed the organic layers with brine, dried over Na2SO4. Removal of the solvent in vacuum left a brown oil (5.01 g) which was purified by silica gel column chromatography with heptane/EtOAc 9:1 to 4:1 to give the title compound as a light yellow solid (2.89 g, 72%). MS (ISP) 403 [(M+H)+]; mp 132° C.

1. temperatureCooled down to 100° C.
2. stirringstirred at 23° C. for 2 h
3. extraction, extracted with EtOAc
4. washwashed the organic layers with brine
5. dry with materialdried over Na2SO4
6. customRemoval of the solvent in vacuum
7. waitleft a brown oil (5.01 g) which
8. customwas purified by silica gel column chromatography with heptane/EtOAc 9:1 to 4:1