2-(2,6-difluorophenyl)acetyl chloride

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 25 ml of methylamine solution (33% in ethanol) are diluted with 90 ml of dichloromethane. While cooling, 9.52 g (50 mmol) of 2,6-difluorophenylacetyl chloride dissolved in 10 ml of dichloromethane are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10°. The reaction mixture is stirred for a further hour at 10° and then extracted three times with water. The organic phase is dried over magnesium sulphate and concentrated. The crude product is recrystallised from dichloromethane/petroleum ether and yields 8.57 g (92.6% of the theoretical yield) of 2,6-difluorophenylacetic acid methylamide of m.p. 163°-164°. While cooling are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10° extracted three times with water The organic phase is dried over magnesium sulphate concentrated The crude product is recrystallised from dichloromethane/petroleum ether yields 8.57 g (92.6% of the

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 75.3 g (0.44 mol) of 2,6-difluorophenylacetic acid are dissolved in 96 ml (156.5 g; 1.32 mol) of thionyl chloride, stirred for 1 hour at 60° and then heated under reflux for 2 hours. The excess thionyl chloride is then distilled off and the residue is fractionated, yielding 79.5 g (95% of the theoretical yield) of 2,6-difluorophenylacetyl chloride. heated under reflux for 2 hours The excess thionyl chloride is then distilled off yielding 79.5 g (95% of the

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 75.3 g (0.44 mol) of 2,6-difluorophenylacetic acid are dissolved in 96 ml (156.5 g; 1.32 mol) of thionyl chloride, stirred for 1 hour at 60° and then heated under reflux for 2 hours. The excess thionyl chloride is then distilled off and the residue is fractionated, yielding 79.5 g (95% of the theoretical yield) of 2,6-difluorophenylacetyl chloride. heated under reflux for 2 hours The excess thionyl chloride is then distilled off yielding 79.5 g (95% of the

反応条件: temp:0.00; pressure:0.00; stir:

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 25 ml of methylamine solution (33% in ethanol) are diluted with 90 ml of dichloromethane. While cooling, 9.52 g (50 mmol) of 2,6-difluorophenylacetyl chloride dissolved in 10 ml of dichloromethane are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10°. The reaction mixture is stirred for a further hour at 10° and then extracted three times with water. The organic phase is dried over magnesium sulphate and concentrated. The crude product is recrystallised from dichloromethane/petroleum ether and yields 8.57 g (92.6% of the theoretical yield) of 2,6-difluorophenylacetic acid methylamide of m.p. 163-164°. While cooling are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10° extracted three times with water The organic phase is dried over magnesium sulphate concentrated The crude product is recrystallised from dichloromethane/petroleum ether yields 8.57 g (92.6% of the

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 75.3 g (0.44 mol) of 2,6-difluorophenylacetic acid are dissolved in 96 ml (156.5 g; 1.32 mol) of thionyl chloride, stirred for 1 hour at 60° and then heated under reflux for 2 hours. The excess thionyl chloride is then distilled off and the residue is fractionated, yielding 79.5 g (95% of the theoretical yield) of 2,6-difluorophenylacetyl chloride. heated under reflux for 2 hours The excess thionyl chloride is then distilled off yielding 79.5 g (95% of the

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 25 ml of methylamine solution (33% in ethanol) are diluted with 90 ml of dichloromethane. While cooling, 9.52 g (50 mmol) of 2,6-difluorophenylacetyl chloride dissolved in 10 ml of dichloromethane are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10°. The reaction mixture is stirred for a further hour at 10° and then extracted three times with water. The organic phase is dried over magnesium sulphate and concentrated. The crude product is recrystallised from dichloromethane/petroleum ether and yields 8.57 g (92.6% of the theoretical yield) of 2,6-difluorophenylacetic acid methylamide of m.p. 163°-164°. While cooling are added dropwise in such a manner that the temperature of the reaction mixture does not exceed 10° extracted three times with water The organic phase is dried over magnesium sulphate concentrated The crude product is recrystallised from dichloromethane/petroleum ether yields 8.57 g (92.6% of the

反応条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: 75.3 g (0.44 mol) of 2,6-difluorophenylacetic acid are dissolved in 96 ml (156.5 g; 1.32 mol) of thionyl chloride, stirred for 1 hour at 60° and then heated under reflux for 2 hours. The excess thionyl chloride is then distilled off and the residue is fractionated, yielding 79.5 g (95% of the theoretical yield) of 2,6-difluorophenylacetyl chloride. heated under reflux for 2 hours The excess thionyl chloride is then distilled off yielding 79.5 g (95% of the