反応 #215701

反応方程式

2-bromo-3,4,5,6-tetrafluorobenzoyl chloride

magnesium chloride

diethyl malonate

hydrochloric acid

triethylamine

→

Diethyl (2-bromo-3,4,5,6-tetrafluoro-benzoyl)malonate

溶媒

acetonitrile

反応条件

後処理

1. 1
   workup.ADDITIONare added dropwise
2. 2
   温度while cooling
3. 3
   workup.STIRRINGthe mixture is subsequently stirred at 0° C. for a further hour
4. 4
   workup.WAITbrought to room temperature overnight
5. 5
   抽出the mixture is extracted three times with methylene chloride
6. 6
   乾燥the extract is dried with Na2SO4
7. 7
   濃縮concentrated in vacuo

実験手順

15.9 g (0.167 mol) of magnesium chloride in 150 ml of anhydrous acetonitrile (dried over zeolite) are initially introduced into the reaction vessel and 26.9 g (0.167 mol) of diethyl malonate are added dropwise, while cooling. The mixture is cooled to 0° C., 46 ml (33.7 g=0.33 mol) of triethylamine are added dropwise and the mixture is subsequently stirred for 30 minutes. 48.9 g (0.168 mol) of 2-bromo-3,4,5,6-tetrafluorobenzoyl chloride are then added dropwise and the mixture is subsequently stirred at 0° C. for a further hour and brought to room temperature overnight. 100 ml of 5N hydrochloric acid are added, the mixture is extracted three times with methylene chloride and the extract is dried with Na2SO4 and concentrated in vacuo.

出典