Reaktion #85460

Reaktionsgleichung

MTBE

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

NaCN

water

→

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

Ausbeute 95.0%

Lösungsmittel

DMSO

DMSO

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.STIRRINGAfter stirring for 30 min
2. 2
   Sonstigethe layers are separated
3. 3
   ExtraktionThe aqueous layer is extracted with MTBE (1.8 vol)
4. 4
   WaschenThe combined organic layers are washed with water (1.8 vol)
5. 5
   Trocknendried (Na2SO4)
6. 6
   Filtrationfiltered
7. 7
   Einengenconcentrated

Vorschrift

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.

Quelle