反应详情

A mixture of 4 cyanobenzoic acid (1.47 g), benzyl mercaptan (1.24 g) and phosphorus pentasulfide (4.44 g) in toluene (40 ml) was refluxed for 20 h. A dark red color was developed immediately after heating. After the reaction was complete (as monitored by GC-MS), it was cooled to room temperature and purified by a column chromatography packed with neutral alumina, eluting with benzene. Removal of the solvent by distillation gave the single compound, benzyl-4-cyanodithiobenzoate (1.15 g, 43%). It was further characterized by 1H and 13C-NMR.

1. temperaturewas refluxed for 20 h
2. temperatureafter heating
3. custompurified by a column chromatography
4. washeluting with benzene
5. customRemoval of the solvent
6. distillationby distillation