Synthetic Route of 24398-88-7, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 24398-88-7 name is Ethyl 3-bromobenzoate, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
To a stirred mixture of a compound of formula V (1 eq), a boronic acid derivative of general formula VI (1.1 eq) and tetrakis(triphenylphosphine)palladium (0.03 eq) in an organic solvent (e.g. 1,2-dimethoxy-ethane) is added at room temperature aqueous 1 M sodium carbonate solution (2.5 eq), the reaction mixture is heated at 80 to 90 C. for around 18 h, cooled, poured into ice-water and extracted two times with ethyl acetate. The combined organic layers are washed two times with brine, dried (e.g. MgSO4) and evaporated. The crude product is further purified by flash chromatography on silica gel (ethyl acetate/n-heptane) and crystallization (e.g. dichloromethane/diethyl ether/n-heptane) to give compounds of general formulae Ia or Ib.Prepared from hexamethyldisilizane (16.5 mL, 79 mmol) and n-BuLi (48.4 mL, 77 mmol) in TBME (40 mL), then commercially available ethyl 3-bromobenzoate (7.55 g, 33 mmol) and tert-butyl acetate (4.86 mL, 36 mmol) in TBME (80 mL) according to the general procedure III. Obtained as a light yellow oil (9.934 g, 101%; 95% purity).
At the same time, in my other blogs, there are other synthetic methods of this type of compound, Ethyl 3-bromobenzoate, and friends who are interested can also refer to it.
Reference:
Patent; Gatti McArthur, Silvia; Wichmann, Juergen; Woltering, Thomas Johannes; US2008/261957; (2008); A1;,
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