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Methyl 5-bromo-4-chloro-2-hydroxybenzoate synthesis

2synthesis methods
-

Yield:55488-81-8 25.3 g

Reaction Conditions:

with sulfuric acid at 70; for 24 h;

Steps:

3a

Taking compound 2 a (35.2 g, 140 mmol) dissolved in methanol (200 ml) in, slowly adding concentrated sulfuric acid (10 ml), 70 °C heating 24 h. TLC monitoring display after the reaction. The reaction liquid concentrated, residue of ethyl acetate (200 ml) dissolved, saturated sodium bicarbonate solution to adjust pH to and 7 - 8, organic phase to saturated salt water (150 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=200:1) purification to obtain compound 3 a (white solid, 25.3 g, yield 68%).

References:

CN109748789,2019,A Location in patent:Paragraph 0063; 0065; 0067

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