反应详情

To TFA (4 mL) at 5° C. the crude 3-[2-chloro-5-(trifluoromethyl)phenyl]-3-[(2,2-diethoxyethyl)amino]prop-2-enenitrile was added. After stirring at room temperature for 30 min, the reaction mixture was concentrated and then diluted with EtOAc and saturated solution of sodium hydrogen carbonate. The organic layer was separated, washed with water and brine, dried over sodium sulfate and concentrated. Column chromatography on silica gel (0 to 20% EtOAc/hexane) afforded the title compound (584 mg, 45% 2 steps).

1. concentrationthe reaction mixture was concentrated
2. additiondiluted with EtOAc and saturated solution of sodium hydrogen carbonate
3. customThe organic layer was separated
4. washwashed with water and brine
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated