反应详情

4-Chlorothiosalicylic acid (2.3 g, 12.2 mmol) and tert-butyl 3-(2-cyano-4-pyridyl)propanoate (1.4 g, 6.0 mmol) were dissolved in pyridine (20 ml), and the mixture was refluxed for 16 hrs. The solvent was evaporated and the residue was subjected to a silica gel column chromatography. The fraction eluted with hexane-ethyl acetate (2:1, v/v) were collected, concentrated and recrystallized from hexane-tetrahydrofuran to give the titled compound (1.3 g, 52%) as white crystals.

1. temperaturethe mixture was refluxed for 16 hrs
2. customThe solvent was evaporated
3. washThe fraction eluted with hexane-ethyl acetate (2:1
4. customv/v) were collected
5. concentrationconcentrated
6. customrecrystallized from hexane-tetrahydrofuran