反应详情

温度

35 °C

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.

1. stirringAfter stirring for 30 min
2. customthe layers are separated
3. extractionThe aqueous layer is extracted with MTBE (1.8 vol)
4. washThe combined organic layers are washed with water (1.8 vol)
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated