Реакция #329313

Уравнение реакции

MTBE

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

NaCN

water

→

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

Выход 95.0%

Растворители

DMSO

DMSO

Условия реакции

Обработка

1. 1
   workup.STIRRINGAfter stirring for 30 min
2. 2
   Другоеthe layers are separated
3. 3
   ЭкстракцияThe aqueous layer is extracted with MTBE (1.8 vol)
4. 4
   ПромывкаThe combined organic layers are washed with water (1.8 vol)
5. 5
   Сушкаdried (Na2SO4)
6. 6
   Фильтрацияfiltered
7. 7
   Концентрированиеconcentrated

Методика

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.

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