methyl 2-bromo-3-oxopentanoate synthesis

Yield:117481-97-7 35%

Reaction Conditions:

with N-Bromosuccinimide;ammonium acetate in tert-butyl methyl ether at 20; for 48 h;

Steps:

Preparation of intermediate J

Preparation of intermediate J NBS (45.1 g, 254 mmol) and NH₄OAc (5.33 g, 69.2 mmol) were added to a solution of methyl-3-oxo valerate (CAS[30414-53-0], 30 g, 231 mmol) in methyl t-butylether (600 mL). The mixture was stirred at room temperature for 48 h. The mixture was filtered and washed with H₂0, dried over Na₂S0₄ and filtered. The filtrate was concentrated under vacuum. The residue was purified by column chromatography over silica gel (eluent: petroleum ether/ethyl acetate 20/1) to give intermediate J (20.0 g, yield: 35%).

References:

WO2017/1660,2017,A1 Location in patent:Page/Page column 41