Synthesis
To a solution of Ethyl acetoacetate (10.0 g, 76.9 mmol, 1 .0 eq) in acetic acid (30 mL) was added bromine (12.3 g, 76.9 mmol, 1 .0 eq) at 0 °C over 10 min. The mixture was stirred at 0 °C for 1 h, the solvent was removed under reduced pressure, and the residue was diluted with water (50 mL). The aqueous mixture was extracted with CH2CI2 (50 mL x 3). The combined organic layers were washed with brine (60 mL x 2), dried over MgS04 and concentrated under reduced pressure to give ethyl 4-bromo-3-oxobutanoate (14.3 g, 85 per cent) as a yellow oil.
References
[1] Patent: CN105820102, 2016, A. Location in patent: Paragraph 0029-0031
[2] Patent: WO2012/63085, 2012, A2. Location in patent: Page/Page column 81
[3] Patent: US2013/225594, 2013, A1. Location in patent: Paragraph 0252; 0253
[4] Canadian Journal of Chemistry, 2001, vol. 79, # 8, p. 1259 - 1271
[5] Patent: TW2016/5831, 2016, A. Location in patent: Paragraph 0211
