反应详情

温度

25 °C

A solution of 3,5-difluorobenzylamine (11.6 g., 0.081 mole) in ether (20 ml.) was added dropwise to a solution of dicyclohexylcarbodiimide (16.7 g., 0.081 mole) and carbon disulfide (32.4 ml., 0.539 mole) in ether (100 ml.) at -5°to -10° C., and the mixture was stirred for 17 hours at 25° C. The mixture was filtered and the solvent was removed under vacuum. The resulting oil was dissolved in hexane-ether (19:1), filtered, and the solvent removed under vacuum. The oil was then dissolved in hexane and purified by flash chromatography (silica) to give 3,5-difluorobenzylisothiocyanate as an oil (5.40 g., 36%).

1. filtrationThe mixture was filtered
2. customthe solvent was removed under vacuum
3. dissolutionThe resulting oil was dissolved in hexane-ether (19:1)
4. filtrationfiltered
5. customthe solvent removed under vacuum
6. dissolutionThe oil was then dissolved in hexane
7. custompurified by flash chromatography (silica)