反应详情

温度

-10 °C

A solution of 3,5-difluorobenzylamine (6.5 g, 0.05 mole) and triethylamine (15.4 ml, 0.11 mole) in 50 ml of tetrahydrofuran was added dropwise to a solution of thiophosgene (4.2 ml, 0.055 mole) in 50 ml of tetrahydrofuran with cooling to -10° C. over a period of twenty minutes. The mixture was stirred at 25° C. for 2.75 hours and then filtered. The filtrate was treated with charcoal, filtered, and evaporated to an oil. The oil was diluted with hexane:ethyl acetate (90:10) and purified on a flash silica column eluted with hexane:ethyl acetate (90:10) to yield 8.0 g (62%) of 3,5-difluorobenzyl isothiocyanate as a yellow oil.

1. filtrationfiltered
2. additionThe filtrate was treated with charcoal
3. filtrationfiltered
4. customevaporated to an oil
5. additionThe oil was diluted with hexane:ethyl acetate (90:10)
6. custompurified on a flash silica column
7. washeluted with hexane:ethyl acetate (90:10)