4-氨基-2,6-二氟苯酚盐酸盐

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 664 mg (3.36 mmol) of 6-chloro-4-nitro-1H-pyrrolo[2,3-b]pyridine (from example XXX), 1.39 g (10.1 mmol) of powdered potassium carbonate and 877 mg (5.04 mmol) of sodium dithionite are suspended in 10 ml of DMSO. The mixture is degassed, and 915 mg (5.04 mmol) of 4-amino-2,6-difluorophenol hydrochloride (from example XXXII) are added. The mixture is heated at 120° C. for 4 hours. After addition of ethyl acetate, the mixture is filtered off with suction through CELITE (diatomaceous earth) and the filtercake is washed with ethyl acetate. The filtrate is extracted three times with sat. sodium bicarbonate solution and with sat. sodium chloride solution. The filtrate is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by column chromatography (silical gel 60, mobile phase: DCM:methanol=50:1). The mixture is degassed the mixture is filtered off with suction through CELITE (diatomaceous earth) the filtercake is washed with ethyl acetate The filtrate is extracted three times with sat. sodium bicarbonate solution The filtrate is dried over sodium sulfate the solvent is removed under reduced pressure The residue is purified by column chromatography (silical gel 60, mobile phase: DCM:methanol=50:1)

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 664 mg (3.36 mmol) of 6-chloro-4-nitro-1H-pyrrolo[2,3-b]pyridine (from example XXX), 1.39 g (10.1 mmol) of powdered potassium carbonate and 877 mg (5.04 mmol) of sodium dithionite are suspended in 10 ml of DMSO. The mixture is degassed, and 915 mg (5.04 mmol) of 4-amino-2,6-difluorophenol hydrochloride (from example XXXII) are added. The mixture is heated at 120° C. for 4 hours. After addition of ethyl acetate, the mixture is filtered off with suction through CELITE (diatomaceous earth) and the filtercake is washed with ethyl acetate. The filtrate is extracted three times with sat. sodium bicarbonate solution and with sat. sodium chloride solution. The filtrate is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by column chromatography (silical gel 60, mobile phase: DCM:methanol=50:1). The mixture is degassed the mixture is filtered off with suction through CELITE (diatomaceous earth) the filtercake is washed with ethyl acetate The filtrate is extracted three times with sat. sodium bicarbonate solution The filtrate is dried over sodium sulfate the solvent is removed under reduced pressure The residue is purified by column chromatography (silical gel 60, mobile phase: DCM:methanol=50:1)

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 664 mg (3.36 mmol) of 6-chloro-4-nitro-1H-pyrrolo[2,3-b]pyridine, 1.39 g (10.1 mmol) of powdered potassium carbonate and 877 mg (5.04 mmol) of sodium dithionite are suspended in 10 ml of DMSO. The mixture is degassed, and 915 mg (5.04 mmol) of 4-amino-2,6-difluorophenol hydrochloride are added. The mixture is heated at 120° C. for 4 hours. After addition of ethyl acetate, the mixture is filtered off with suction through celite, and the celite is washed with ethyl acetate. The filtrate is shaken three times with saturated sodium bicarbonate solution and with saturated, sodium chloride solution. The filtrate is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by column chromatography (silica gel 60, mobile phase: dichloromethane/methanol=50:1). The mixture is degassed the mixture is filtered off with suction through celite the celite is washed with ethyl acetate The filtrate is dried over sodium sulfate the solvent is removed under reduced pressure The residue is purified by column chromatography (silica gel 60, mobile phase: dichloromethane/methanol=50:1)

反应条件: temp:120.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

实验步骤: 664 mg (3.36 mmol) of 6-chloro-4-nitro-1H-pyrrolo[2,3-b]pyridine (from example XXX), 1.39 g (10.1 mmol) of powdered potassium carbonate and 877 mg (5.04 mmol) of sodium dithionite are suspended in 10 ml of DMSO. The mixture is degassed, and 915 mg (5.04 mmol) of 4-amino-2,6-difluorophenol hydrochloride (from example XXXII) are added. The mixture is heated at 120° C. for 4 hours. After addition of ethyl acetate, the mixture is filtered off with suction through CELITE (diatomaceous earth) and the filtercake is washed with ethyl acetate. The filtrate is extracted three times with sat. sodium bicarbonate solution and with sat. sodium chloride solution. The filtrate is dried over sodium sulfate and the solvent is removed under reduced pressure. The residue is purified by column chromatography (silical gel 60, mobile phase: DCM:methanol=50:1). The mixture is degassed the mixture is filtered off with suction through CELITE (diatomaceous earth) the filtercake is washed with ethyl acetate The filtrate is extracted three times with sat. sodium bicarbonate solution The filtrate is dried over sodium sulfate the solvent is removed under reduced pressure The residue is purified by column chromatography (silical gel 60, mobile phase: DCM:methanol=50:1)