Preparation methods of Methyl salicylate (CAS#: 119-36-8) from TNJ Chemical
Wintergreen oil is one of the natural fragrances. Its main component is methyl salicylate （CAS No.: 119-36-8）, which can be obtained by esterification of salicylic acid (ortho-hydroxybenzoic acid) and methanol as raw materials under the catalysis of concentrated sulfuric acid.
Ⅰ. As shown in the figure, in a 100mL three-necked flask, put 6.9g (0.05mol) salicylic acid and 24g (30mL, 0.75mol) methanol, add about 10mL toluene to the mixture, then carefully add 8mL concentrated sulfuric acid, shake and mix: add 1~2 zeolite, install reflux condenser to keep 85-95℃ on the asbestos net, heat to reflux for 1.5-2 hours:
Ⅱ. After the device is cooled, separate methanol, add 50mL of water to the flask, then transfer to the separatory funnel, separate the lower product, discard the upper aqueous layer, and pour the organic layer into the separatory funnel; use 50mL 5% in turn Wash once with NaHCO3 solution (the solution is weakly alkaline), and once with 30 mL of water (the products are all in the lower layer), and the organic layer will get the crude ester;
Ⅲ. The crude ester was distilled, and the fractions at 221℃～224℃ were collected. The product is weighed after being dried by 0.5g anhydrous CaCl2.
It is known that an azeotrope formed by toluene and water has a boiling point of 85°C. The addition of toluene in this experiment can easily evaporate water.
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