反应详情

A mixture of 4-chloro-2-mercaptobenzoic acid (3.0 g, 15.9 mmol), 2-cyano-4-methylpyridine (1.9 g, 16.0 mmol) and pyridine (15 ml) was refluxed for 9 hrs as described in Example 9. After cooling, the precipitated crystals were collected by filtration, subjected to a silica gel column chromatography, eluted with ethyl acetate-methanol (5:1, v/v) and recrystallized from chlorobenzene-hexane to give the titled compound (1.47 g, 32%)

1. temperaturewas refluxed for 9 hrs
2. temperatureAfter cooling
3. filtrationthe precipitated crystals were collected by filtration
4. washeluted with ethyl acetate-methanol (5:1
5. customv/v) and recrystallized from chlorobenzene-hexane