反应详情

Lead thiocyanate (45 g, 139 mmol) was added in portions to a stirred solution of chlorine (20.3 g, 290 mmol) in anhydrous acetic acid (600 ml) under an atmosphere of argon. The mixture was stirred for 15 minutes. 1,2-Methylenedioxybenzene (35 g, 286 mmol) was added in one portion. The mixture was stirred for 1 hour and then filtered. The filtrate was added to ice-water (3.5 liters). The precipitated solid was collected by filtration, dissolved in ethyl acetate and dried (MgSO4). The solvent was removed by evaporation to give 3,4-methylenedioxyphenyl thiocyanate as a pale green oil (40.3 g, 79% yield). The oil solidified and was used without further purification or characterisation.

1. stirringThe mixture was stirred for 1 hour
2. filtrationfiltered
3. additionThe filtrate was added to ice-water (3.5 liters)
4. filtrationThe precipitated solid was collected by filtration
5. dissolutiondissolved in ethyl acetate
6. dry with materialdried (MgSO4)
7. customThe solvent was removed by evaporation