反应详情

tert-Butyl 3-(2-cyano-4-pyridyl)propanoate (1.3 g, 5.6 mmol) and 4-bromothiosalicylic acid (1.8 g, 8.0 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 (3:2, v/v) were collected, concentrated and recrystallized from hexane-tetrahydrofuran to give the titled compound (0.63 g, 25%) as white crystals.

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