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ChemicalBook CAS DataBase List Methyl 5-broMo-2-(difluoroMethoxy)benzoate
1131587-78-4

Methyl 5-broMo-2-(difluoroMethoxy)benzoate synthesis

2synthesis methods
-

Yield:1131587-78-4 50%

Reaction Conditions:

with potassium carbonate in N,N-dimethyl-formamide at 80; for 24 h;

Steps:

121.1

To a solution of methyl 5-bromo-2-hydroxybenzoate (409 mg, 1.77 mmol) in DMF (5 mL) was added potassium carbonate (367 mg, 2.67 mmol) and ethyl 2-bromo-2,2-difluoroacetate (280 μ^, 2.13 mmol). The resulting mixture was heated at 80 °C for 24 hrs. The resulting solution was cooled to RT, diluted with ether and washed sequentially with water, 10% aq. HCl, water and brine. The organic extract was then dried over Na2S04, filtered and the filtrate concentrated in vacuo. Further purification by way of column chromatography (S1O2, gradient elution, Hex to 2:1 (v/v) Hex: EtOAc) afforded methyl 5-bromo-2- (difluoromethoxy)benzoate as a yellow oil (250 mg, 50% yield).

References:

WO2013/134562,2013,A1 Location in patent:Paragraph 00294

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