METHYL ABIETATE CAS 127-25-3

Add 30mL organic solvent DMF in the 250mL three-neck flask equipped with stirrer, thermometer and reflux condenser, then add abietic acid (0.05mol, 15.0g) and methylation reagent dimethyl carbonate C3H6O3 (0.5mol, 45.0g ), alkali catalyst lithium hydroxide LiOH H O (0.1mol, 4.2g), make abietic acid, dimethyl carbonate, lithium hydroxide dissolve in DMF, under nitrogen protection, be heated to stable reflux in 100 ℃ of oil baths, i.e. When the number of reflux drops in the three-necked bottle is 1 to 2 drops/second, it is stable, and the stable reflux temperature is 93°C. The progress of the reaction was tracked by thin-layer chromatography every 1 hour until it was detected that there was no reaction raw material in the three-necked flask, and the reaction was terminated, and the reaction lasted for 46 hours. After the reaction was finished, pour the contents of the reaction into a beaker with 600 mL of deionized water, adjust the pH to neutral with 3.5% hydrochloric acid solution, then extract with 50 mL of dichloromethane, take the organic phase, and use the remaining water phase with two Chloromethane extraction, repeated extraction 3 times in total, combined the organic phase obtained 3 times, added deionized water to wash the extract, separated the organic layer and dried it with anhydrous sodium sulfate. The crude product of METHYL ABIETATE was obtained. The content of methyl abietic acid in the crude product was detected by liquid phase. Finally, the crude product of METHYL ABIETATE is concentrated to dryness under reduced pressure, and through column chromatography (silica gel column 300-400 mesh, gradient elution is carried out with composition being 100% petroleum ether) to obtain 15.6 g of the product methyl abietate, the yield is 99.6 %. By using dimethyl carbonate as the METHYL ABIETATE reagent, the yield of METHYL ABIETATE is very high, reaching 99.6%.