2-溴-N-(2,4-二氟苯基)乙酰胺

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: WSC (2.1 g, 11 mmols) and HOBt (1.49 g, 11 mmols) were added to a DMF (30 ml) solution of 2,4-difluoroaniline (1.29 g, 10 mmols) and bromoacetic acid (2.08 g, 15 =mmols), and stirred at room temperature for 12 hours. The reaction mixture was extracted with other. The organic layer was washed with water, 1 N HCl, an aqueous saturated solution of sodium hydrogencarbonate and saturated saline in that order, and dried with anhydrous magnesium sulfate, and the solvent was evaporated. Then, the residue was purified through silica gel column chromatography (developer:hexane/acetone=5/1), and the resulting crystals were recrystallized from ether-hexane to obtain 1.7 g (yield: 68%) of 2-bromo-N-(2,4-difluorophenyl)acetamide, as colorless needle-like crystals. The reaction mixture was extracted with other The organic layer was washed with water, 1 N HCl an aqueous saturated solution of sodium hydrogencarbonate and saturated saline in that order, and dried with anhydrous magnesium sulfate the solvent was evaporated Then, the residue was purified through silica gel column chromatography (developer:hexane/acetone=5/1) the resulting crystals were recrystallized from ether-hexane

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: WSC (2.1 g, 11 mmols) and HOBt (1.49 g, 11 mmols) were added to a DMF (30 ml) solution of 2,4-difluoroaniline (1.29 g, 10 mmols) and bromoacetic acid (2.08 g, 15 =mmols), and stirred at room temperature for 12 hours. The reaction mixture was extracted with other. The organic layer was washed with water, 1 N HCl, an aqueous saturated solution of sodium hydrogencarbonate and saturated saline in that order, and dried with anhydrous magnesium sulfate, and the solvent was evaporated. Then, the residue was purified through silica gel column chromatography (developer:hexane/acetone=5/1), and the resulting crystals were recrystallized from ether-hexane to obtain 1.7 g (yield: 68%) of 2-bromo-N-(2,4-difluorophenyl)acetamide, as colorless needle-like crystals. The reaction mixture was extracted with other The organic layer was washed with water, 1 N HCl an aqueous saturated solution of sodium hydrogencarbonate and saturated saline in that order, and dried with anhydrous magnesium sulfate the solvent was evaporated Then, the residue was purified through silica gel column chromatography (developer:hexane/acetone=5/1) the resulting crystals were recrystallized from ether-hexane

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: WSC (2.1 g, 11 mmols) and HOBt (1.49 g, 11 mmols) were added to a DMF (30 ml) solution of 2,4-difluoroaniline (1.29 g, 10 mmols) and bromoacetic acid (2.08 g, 15 =mmols), and stirred at room temperature for 12 hours. The reaction mixture was extracted with other. The organic layer was washed with water, 1 N HCl, an aqueous saturated solution of sodium hydrogencarbonate and saturated saline in that order, and dried with anhydrous magnesium sulfate, and the solvent was evaporated. Then, the residue was purified through silica gel column chromatography (developer:hexane/acetone=5/1), and the resulting crystals were recrystallized from ether-hexane to obtain 1.7 g (yield: 68%) of 2-bromo-N-(2,4-difluorophenyl)acetamide, as colorless needle-like crystals. The reaction mixture was extracted with other The organic layer was washed with water, 1 N HCl an aqueous saturated solution of sodium hydrogencarbonate and saturated saline in that order, and dried with anhydrous magnesium sulfate the solvent was evaporated Then, the residue was purified through silica gel column chromatography (developer:hexane/acetone=5/1) the resulting crystals were recrystallized from ether-hexane

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 4 g (16 mmol) of the bromoacetanilide from Example I and 4.2 g (19 mmol) of 4-(2-oxo-1-benzimidazolinyl)piperidine in 50 ml of dimethylformamide are stirred at RT for 18 h with 2.6 g (19 mmol) of potassium carbonate. The solid is then filtered off with suction, the filtrate is partitioned between ethyl acetate and water, and the aqueous phase is extracted 3 times with ethyl acetate. The organic phases are combined, washed with saturated sodium chloride solution, dried (MgSO4) and concentrated. The residue obtained is triturated with ether, and the solid is filtered off and then recrystallized from methanol. The solid is then filtered off with suction the filtrate is partitioned between ethyl acetate and water the aqueous phase is extracted 3 times with ethyl acetate washed with saturated sodium chloride solution dried (MgSO4) concentrated The residue obtained is triturated with ether the solid is filtered off recrystallized from methanol

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 5.16 g (40 mmol) of 2,4-difluoroaniline and 6.3 g (40 mmol) of bromoacetyl chloride are treated in 200 ml of dichloromethane with 5.17 g (40 mmol) of Hunig base. After 4 h, the mixture is washed twice with 1N hydrochloric acid and once with water, dried (MgSO4) and concentrated. the mixture is washed twice with 1N hydrochloric acid and once with water dried (MgSO4) concentrated

反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: WSC (2.1 g, 11 mmols) and HOBt (1.49 g, 11 mmols) were added to a DMF (30 ml) solution of 2,4-difluroaniline (1.29g, 10 mmols) an bromoacetic acid (2.08 g, 15 mmols), and stirred at room temperature for 12 hours. The reaction mixture was extracted with ether. The organic layer was washed with water, 1 N HCl, an aqueous saturated solution of sodium hydrogencarbonate and saturated saline in that order, and dried with anhydrous magnesium sulfate, and the solvent was evaporated. Then, the residue was purified through silica gel column chromatography (developer: hexane/acetone=5/1), and the resulting crystals were recrystallized from ether-hexane to obtain 1.7 g (yield: 68%) of 2-bromo-N-(2,4-difluorophenyl)acetamide as colorless needle-like crystals. The reaction mixture was extracted with ether The organic layer was washed with water, 1 N HCl an aqueous saturated solution of sodium hydrogencarbonate and saturated saline in that order, and dried with anhydrous magnesium sulfate the solvent was evaporated Then, the residue was purified through silica gel column chromatography (developer: hexane/acetone=5/1) the resulting crystals were recrystallized from ether-hexane