반응 #1908820

반응 방정식

ammonium chloride

aminonitrile

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

4-fluorophenyl magnesium bromide

water

→

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

용매

THF

THF

반응 조건

후처리

1. 1
   온도while cooling with ice
2. 2
   workup.ADDITIONwere added
3. 3
   온도while cooling with ice
4. 4
   추출the mixture was extracted with diethyl ether (3×100 ml)
5. 5
   세척The organic phase was washed with water and saturated sodium chloride solution
6. 6
   건조dried (Na2SO4)
7. 7
   농축concentrated by evaporation

실험 절차

A solution of the aminonitrile 12 (19.89 g, 88 mmole) in absolute THF (160 ml) was added dropwise to a 1M solution of 4-fluorophenyl magnesium bromide in THF (220 ml, 220 mmole) under argon and while cooling with ice, 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.

출처