反应详情

4-Fluorothiosalicylic acid (1.9 g, 11.3 mmol) and tert-butyl 3-(2-cyano-4-pyridyl)propanoate (1.3 g, 5.6 mmol) were dissolved in pyridine (20 ml), and the mixture was refluxed for 18 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with hexane-ethyl acetate (2:1, v/v) were collected, concentrated and recrystallized from hexane-tetrahydrofuran to give the titled compound (1.2 g, 54%) as white crystals.

1. temperaturethe mixture was refluxed for 18 hrs
2. customThe solvent was evaporated
3. washThe fractions eluted with hexane-ethyl acetate (2:1
4. customv/v) were collected
5. concentrationconcentrated
6. customrecrystallized from hexane-tetrahydrofuran