反应详情

温度

40 °C

Potassium thiocyanate (11.03 g, 114 mmol) was suspended in acetone (63.1 mL) and heated to 40° C. under nitrogen atmosphere. To this was added 3-fluorobenzoyl chloride (11.35 mL, 95 mmol), and the resulting mixture was stirred at 50° C. for 6 hours. The heterogeneous mixture was filtered, and the solid was further washed with acetone. The filtrate was concentrated and purified by silica gel chromatography (10% EtOAc/Hexanes as the eluent) to afford 3-fluorobenzoyl isothiocyanate (6.5 g, 37.9% yield) as a light orange oil.

1. filtrationThe heterogeneous mixture was filtered
2. washthe solid was further washed with acetone
3. concentrationThe filtrate was concentrated
4. custompurified by silica gel chromatography (10% EtOAc/Hexanes as the eluent)