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METHYL 5-BROMO-2-HYDROXY-4-METHOXYBENZOATE synthesis

4synthesis methods
-

Yield:39503-52-1 456 mg

Reaction Conditions:

with sulfuric acid in methanol at 70; for 24 h;

Steps:

12

Taking compound 2 d (1.0 g, 4.1 mmol) dissolved in methanol (10 ml) in, slowly adding concentrated sulfuric acid (3 ml), 70 °C heating 24 h. TLC monitoring display after the reaction. The reaction liquid concentrated, residue of ethyl acetate (20 ml) dissolved, saturated sodium bicarbonate solution to adjust pH to and 7 - 8, organic phase to saturated salt water (15 ml x 2) washing, drying with anhydrous sodium sulfate. Evaporate the solvent under reduced pressure. The residue by silica gel column chromatography (petroleum ether: ethyl acetate=50:1) purification to obtain compound 3 d (white solid, 456 mg, yield 44%).

References:

CN109748789,2019,A Location in patent:Paragraph 0125; 0127; 0129

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