Реакция #40920

Уравнение реакции

ammonium chloride

4-fluorophenyl magnesium bromide

aminonitrile

Dimethylamino-(1,4-dioxa-spiro[4.5]dec-8-yl)-acetonitrile

water

→

(1,4-dioxa-spiro[4.5]dec-8-yl-4-fluorophenylmethyl]-dimethylamine

Растворители

THF

THF

Условия реакции

Обработка

1. 1
   workup.ADDITIONwere added
2. 2
   Температураwhile cooling with ice
3. 3
   Экстракцияthe mixture was extracted with diethyl ether (3×100 ml)
4. 4
   ПромывкаThe organic phase was washed with water and saturated sodium chloride solution
5. 5
   Сушкаdried (Na2SO4)
6. 6
   Концентрированиеconcentrated by evaporation

Методика

A solution of the aminonitrile 6 (19.89 g 88 mmole) in absolute THF (160 ml) was added dropwise under argon and cooling with ice to a 1M solution of 4-fluorophenyl magnesium bromide in THF (220 ml, 220 mmole) and stirred for 20 hours at RT. To work up the reaction mixture, saturated ammonium chloride solution (100 ml) and water (100 ml) were added while cooling with ice, and the mixture was extracted with diethyl ether (3×100 ml). The organic phase was washed with water and saturated sodium chloride solution, dried (Na2SO4) and concentrated by evaporation.

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