反应详情

tert-Butyl 3-(6-cyano-2-pyridyl)propanoate (1.5 g, 6.5 mmol) and 4-fluorothiosalicylic acid (1.7 g, 9.7 mmol) were dissolved in pyridine (10 ml), and the mixture was refluxed for 15 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with hexane-ethyl acetate (3:1, v/v) were collected, concentrated and recrystallized from hexane-ethyl acetate to give the titled compound (1.36 g, 54%) as white crystals.

1. temperaturethe mixture was refluxed for 15 hrs
2. customThe solvent was evaporated
3. washThe fractions eluted with hexane-ethyl acetate (3:1
4. customv/v) were collected
5. concentrationconcentrated
6. customrecrystallized from hexane-ethyl acetate