Reacción #169518

Ecuación de reacción

MTBE

5-chloromethyl-2,2-difluoro-1,3-benzodioxole

NaCN

water

→

(2,2-difluoro-1,3-benzodioxol-5-yl)-acetonitrile

Rendimiento 95.0%

Disolventes

DMSO

DMSO

Condiciones de reacción

Tratamiento posterior

1. 1
   workup.STIRRINGAfter stirring for 30 min
2. 2
   Otrothe layers are separated
3. 3
   ExtracciónThe aqueous layer is extracted with MTBE (1.8 vol)
4. 4
   LavadoThe combined organic layers are washed with water (1.8 vol)
5. 5
   Secadodried (Na2SO4)
6. 6
   Filtraciónfiltered
7. 7
   Concentraciónconcentrated

Procedimiento

A solution of 5-chloromethyl-2,2-difluoro-1,3-benzodioxole (1 eq) in DMSO (1.25 vol) is added to a slurry of NaCN (1.4 eq) in DMSO (3 vol) maintaining the temperature between 30-40° C. The mixture is stirred for 1 hour then water (6 vol) is added followed by MTBE (4 vol). After stirring for 30 min, the layers are separated. The aqueous layer is extracted with MTBE (1.8 vol). The combined organic layers are washed with water (1.8 vol), dried (Na2SO4), filtered, and concentrated to afford crude (2,2-difluoro-1,3-benzodioxol-5-yl)-acetonitrile (95%) that is used directly in the next step.

Fuente