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Methyl 2-bromo-4-fluoro-5-methoxybenzoate synthesis

2synthesis methods
-

Yield:1007455-22-2 100%

Reaction Conditions:

with sulfuric acid for 7.5 h;Reflux;

Steps:

59 EXAMPLE 59 Methyl 2-bromo-4-fluoro-5-methoxybenzoate

A solution of 9-2 (1 g, 4.03 mmol) and 96% H2SO4 (0.65 mL, 13 mmol) in dry MeOH (15 mL) was refluxed for 7.5 h and cooled to rt. MeOH was evaporated and the residue taken up in DCM (15 mL), washed with saturated sodium bicarbonate (15 mL). The separated aqueous phase (final pH 7.5-8) was extracted with DCM (2×10 mL) and the organic phases were combined and washed with water (15 mL). The resulting organic phase was dried over sodium sulfate, concentrated to yield 9-3 as a solid (1.06 g, 100% yield). HPLC 98% pure.

References:

US2015/175540,2015,A1 Location in patent:Paragraph 0368; 0371; 0372