반응 #1732574

반응 방정식

ammonium chloride

THF

3-fluorophenylmagnesium bromide

THF

aminonitrile

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

→

[(1,4-Dioxa-spiro[4.5]dec-8-yl)-3-fluorophenyl-methyl]-dimethylamine

용매

water

반응 조건

후처리

1. 1
   온도while cooling with ice
2. 2
   온도while cooling with ice
3. 3
   추출extracting the mixture with diethyl ether (3×100 ml)
4. 4
   세척The organic phase was washed with water and saturated sodium chloride solution
5. 5
   기타dried
6. 6
   농축concentrated

실험 절차

A solution of the aminonitrile 4 (23.45 g, 104 mmol) in absol. THF (100 ml) was added dropwise to a 1 M solution of 3-fluorophenylmagnesium bromide in THF (208 ml, 208 mmol) under argon and while cooling with ice, and the mixture was stirred at RT for 20 hours. The reaction mixture was worked up by adding saturated ammonium chloride solution (100 ml) and water (100 ml) while cooling with ice, and extracting the mixture with diethyl ether (3×100 ml). The organic phase was washed with water and saturated sodium chloride solution, dried and concentrated.

출처