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ChemicalBook CAS DataBase List methyl 4-bromo-3-oxo-butanoate

methyl 4-bromo-3-oxo-butanoate synthesis

8synthesis methods
-

Yield: 96.3%

Reaction Conditions:

with bromine in ethyl acetate

Steps:

1; 2; 3; 4 Embodiment 3
At a flow rate of 270 mL/min and 260 mL/min, two constant-flow pumps were used to inject bromine at a concentration of 2.5 mol/L into the two inlets of the polytetrafluoroethylene microreactor at -5 °C. The ethyl acetate solution and the diketene in ethyl acetate solution were mixed for 16 s, and the reaction was completed. The resulting effluent was transferred to the next -5 °C polytetrafluoroethylene microreactor while passing through a constant flow pump at 265 mL/min. The volumetric flow rate is input to methanol at the other inlet of the microreactor. After the reaction system is allowed to stand for 2.5 minutes, the obtained effluent is transferred to a conventional reaction vessel for rectification and purification, and ethyl acetate, methanol and the like are recovered for application, and 122.07 g of 4-bromo is obtained. Methyl acetoacetate (yield 96.3%, purity 99.14%)

References:

University of Jinan;Wang Bin;Zheng Gengxiu;Gao Lingfeng;Sun Wei;Li Min;Zheng Guangbing CN110143873, 2019, A Location in patent:Paragraph 0117-0020