反应详情

tert-Butyl 2-(2-cyano-4-pyridyl)ethylcarbamate (3.0 g, 12 mmol) and methyl thiosalicylate (3.6 g, 21 mmol) were dissolved in toluene (12 ml), and triethylamine (6.0 ml, 43 mmol) was added thereto. The mixture was refluxed for 8 hrs. The solvent was evaporated, and the residue was subjected to a silica gel column chromatography. The fractions eluted with ethyl acetate-hexane (2:1, v/v) were collected, concentrated and recrystallized from hexane-ethanol to give the titled compound (3.3 g, 71%) as white crystals.

1. temperatureThe mixture was refluxed for 8 hrs
2. customThe solvent was evaporated
3. washThe fractions eluted with ethyl acetate-hexane (2:1
4. customv/v) were collected
5. concentrationconcentrated
6. customrecrystallized from hexane-ethanol