تفاعل #85460

معادلة التفاعل

MTBE

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

NaCN

water

→

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

المردود 95.0%

المذيبات

DMSO

DMSO

ظروف التفاعل

المعالجة

1. 1
   workup.STIRRINGAfter stirring for 30 min
2. 2
   أخرىthe layers are separated
3. 3
   استخلاصThe aqueous layer is extracted with MTBE (1.8 vol)
4. 4
   غسيلThe combined organic layers are washed with water (1.8 vol)
5. 5
   تجفيفdried (Na2SO4)
6. 6
   ترشيحfiltered
7. 7
   تركيزconcentrated

الإجراء التجريبي

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.

المصدر