反応 #169518

反応方程式

MTBE

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

NaCN

water

→

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

収率 95.0%

溶媒

DMSO

DMSO

反応条件

後処理

1. 1
   workup.STIRRINGAfter stirring for 30 min
2. 2
   その他the layers are separated
3. 3
   抽出The aqueous layer is extracted with MTBE (1.8 vol)
4. 4
   洗浄The combined organic layers are washed with water (1.8 vol)
5. 5
   乾燥dried (Na2SO4)
6. 6
   ろ過filtered
7. 7
   濃縮concentrated

実験手順

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.

出典