反应详情

温度

60 °C

3.9 g (0.16 mol) of magnesium are initially introduced into 8.6 ml of ethanol and the reaction is started with carbon tetrachloride. A solution of 23.1 g (0.144 mol) of diethyl malonate in 16.3 ml of ethanol is added dropwise at an internal temperature of 50°-60° C. such that this temperature is maintained. The mixture is then subsequently stirred at 60° C. for one hour. Thereafter, a solution of 31.3 g (0.148 mol) of 3-chloro-2,4-difluorobenzoyl chloride in 16 ml of toluene is added dropwise at -10° to -5° C. and the mixture is subsequently stirred at 0° C. for one hour and then overnight, while warming to room temperature. The reaction mixture is poured onto ice-water, acidified with 10 ml of concentrated sulphuric acid and extracted with toluene. The extract is washed with saturated sodium chloride solution and the solvent is removed in vacuo.

1. temperatureis maintained
2. stirringthe mixture is subsequently stirred at 0° C. for one hour
3. temperatureovernight, while warming to room temperature
4. additionThe reaction mixture is poured onto ice-water
5. extractionextracted with toluene
6. washThe extract is washed with saturated sodium chloride solution
7. customthe solvent is removed in vacuo