ethyl 3-(3,5-difluoroanilino)-2-methyl-3-oxopropanoate

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

実験手順: Prepared according to procedure B using ethyl 3-(3,5-difluorophenylamino)-2-methyl-3-oxopropanoate (11.4 g, 44.3 mmol) (described herein) in THF (40 mL), and sodium hydroxide (1.22 g, 53.2 mmol) in water (10 mL). The reaction was stirred at rt for 2 h, affording 3-(3,5-difluorophenylamino)-2-methyl-3-oxopropanoic acid. Mass Spectrum (ESI) m/e=230 (M+1). Prepared

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Prepared according to procedure A using diethyl 2-methylmalonate (34.5 mL, 205 mmol), pyridine (15.6 mL, 190 mmol), and 3,5-difluorobenzenamine (12.4 g, 96 mmol). The reaction was heated to 130° C. for 2 days. Purification afforded ethyl 3-(3,5-difluorophenylamino)-2-methyl-3-oxopropanoate. Mass Spectrum (ESI) m/e=258 (M+1). Prepared Purification

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

実験手順: Prepared according to Procedure B using ethyl 3-(3,5-difluorophenylamino)-2-methyl-3-oxopropanoate (11.4 g, 44.3 mmol; described herein) in THF (40 mL), and sodium hydroxide (1.22 g, 53.2 mmol) in water (10 mL). The reaction was stirred at rt for 2 h, affording 3-(3,5-difluorophenylamino)-2-methyl-3-oxopropanoic acid. Mass Spectrum (ESI) m/e=230.0 (M+1). Prepared

反応条件: temp:130.01; pressure:0.00; stir:; See reaction.notes.procedure_details.

実験手順: Prepared according to Procedure A using diethyl 2-methylmalonate (34.5 mL, 205 mmol), pyridine (15.6 mL, 190 mmol), and 3,5-difluorobenzenamine (12.4 g, 96 mmol). The reaction was heated to 130° C. for 2 days. Purification afforded ethyl 3-(3,5-difluorophenylamino)-2-methyl-3-oxopropanoate. Mass Spectrum (ESI) m/e=258.2 (M+1). Prepared Purification