反应详情

tert-Butyl 3-(6-cyano-4-methyl-2-pyridyl)propanoate (0.72 g, 2.9 mmol) and methyl thiosalicylate (0.99 g, 5.9 mmol) were dissolved in toluene (4 ml), and triethylamine (2.0 ml, 14.3 mmol) was added thereto. The mixture was refluxed for 14 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with ethyl acetate-hexane (1:2, v/v) were collected, concentrated and recrystallized from ethyl acetate-hexane to give the titled compound (0.61 g, 54%) as white crystals.

1. temperatureThe mixture was refluxed for 14 hrs
2. customThe solvent was evaporated
3. washThe fractions eluted with ethyl acetate-hexane (1:2
4. customv/v) were collected
5. concentrationconcentrated
6. customrecrystallized from ethyl acetate-hexane