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88466-30-2

2-HYDROXY-3-PROPIONYL-BENZOIC ACID METHYL ESTER synthesis

2synthesis methods
-

Yield:88466-30-2 81%

Reaction Conditions:

Stage #1: propionyl chloride;methyl salicylate in carbon disulfide at 40; for 4 h;
Stage #2: with titanium(IV) tetrachloride in carbon disulfide; for 0.5 h;Fries Phenol Ester Rearrangement;Solvent;

Steps:

1.1; 2.1; 3.1 first step, the preparation of methyl 3-propionyl salicylate

Add 30.4g (0.2mol) methyl salicylate and 200ml carbon disulfide to a 500ml four-necked flask, turn on stirring, slowly drop in 20.4g (0.24mol) of propionyl chloride after the solids are all dissolved, heat up to 40°C, and keep the reaction 4h, add 38.0g (0.2mol) titanium tetrachloride and stir for 0.5h, evaporate the solvent under reduced pressure, heat up to 120 °C for 4h reaction, add ice water to quench the reaction, and distill the oily substance under reduced pressure to obtain 3-propionylsalicylic acid Methyl ester 33.6g, yield 81%.

References:

CN114736183,2022,A Location in patent:Paragraph 0004; 0011; 0014; 0017