反应详情

tert-Butyl 2-(2-cyano-4-pyridyl)ethylcarbamate (1.5 g, 6.0 mmol) and 4-chlorothiosalicylic acid (2.3 g, 12.1 mmol) were dissolved in pyridine (10 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 (1:1, v/v) were collected, concentrated and recrystallized from hexane-tetrahydrofuran to give the titled compound (0.48 g, 19%) as white crystals.

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