Reacción #552686

Ecuación de reacción

Lead thiocyanate

chlorine

1,2-Methylenedioxybenzene

→

3,4-methylenedioxyphenyl thiocyanate

Rendimiento 161.8%

Disolventes

acetic acid

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGThe mixture was stirred for 1 hour
2. 2
   Filtraciónfiltered
3. 3
   workup.ADDITIONThe filtrate was added to ice-water (3.5 liters)
4. 4
   FiltraciónThe precipitated solid was collected by filtration
5. 5
   workup.DISSOLUTIONdissolved in ethyl acetate
6. 6
   Secadodried (MgSO4)
7. 7
   OtroThe solvent was removed by evaporation

Procedimiento

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.

Fuente