반응 #85460

반응 방정식

MTBE

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

NaCN

water

→

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

수율 95.0%

용매

DMSO

DMSO

반응 조건

후처리

1. 1
   workup.STIRRINGAfter stirring for 30 min
2. 2
   기타the layers are separated
3. 3
   추출The aqueous layer is extracted with MTBE (1.8 vol)
4. 4
   세척The combined organic layers are washed with water (1.8 vol)
5. 5
   건조dried (Na2SO4)
6. 6
   여과filtered
7. 7
   농축concentrated

실험 절차

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.

출처