tetradecyl methacrylate synthesis

Yield:-

Reaction Conditions:

with toluene-4-sulfonic acid;hydroquinone in toluene at 60;Reflux;

Steps:

1 Example 1
2) In a 500 mL four-necked flask equipped with a thermocouple, a stirrer, a water separator, and a reflux condenser,Add an appropriate amount of tetradecanol, toluene (solvent), hydroquinone (polymerization inhibitor), and p-toluenesulfonic acid (catalyst), and heat them to 60°C to completely dissolve them.Then add a methacrylic acid so that the molar ratio of methacrylic acid and tetradecanol is 1:1, the amount of toluene is 75% of the total mass of methacrylic acid and tetradecanol, and the amount of hydroquinone is methacrylic acid and The total mass of tetradecanol is 0.5%, and the amount of p-toluenesulfonic acid is 1.0% of the total mass of methacrylic acid and tetradecanol; 3) continue to heat up to the reflux temperature, the water generated by the reaction carried by the water-bearing agent toluene, in the water separator layer;4) When the reaction reaches the theoretical amount of water, the reaction is completed, the reaction is stopped, excess methacrylic acid and toluene are distilled off under reduced pressure, washed with a mass fraction of 5% alkalinity until the lower aqueous layer is colorless, and then saturated NaCl is used. The solution was washed to neutrality and the pH was 7;5) Take an appropriate amount of anhydrous calcium chloride to dry the product, suction filtration, and vacuum drying in a vacuum oven for more than 48 hours to obtain pure tetradecyl methacrylate.

References:

Shanxi Jujiehan Chemical Co., Ltd.;Li Changying CN107903174, 2018, A Location in patent:Paragraph 0010; 0011; 0012; 0013