Yield:-

Reaction Conditions:

with H-type zeolite catalyst at 60 - 120; under 760.051 Torr; for 2.83333 h;Sealed tube;Inert atmosphere;Reagent/catalyst;

Steps:

1. Reaction experiment
Acetyltriethyl citrate was prepared through a solid-liquid reaction.55.3 g (0.2 M) of triethyl citrate and 24.5 g (0.28 M) of acetic anhydride were mixed with 0.5 g of a solid catalyst and reacted.The reactor used was a batch reactor equipped with a condenserFirst, the reactants were fed into a reactor capable of temperature maintenance and magnetic stirring. Then, nitrogen was injected into the reactor so that the pressure inside the reactor was 1 atm to remove the air inside the reactor into which the reactants were injected and replace with nitrogen. After the reactor was sealed with nitrogen, the internal temperature of the reactor was raised to 60 DEG C, and the reactor was stirred at 500 rpm for 20 minutes to mix the reactants. After the primary agitation, the inlet of the reactor was opened and solid acid catalyst was injected, and the reactor was sealed. The internal temperature of the closed reactor was raised to 145 and kept constant, followed by 2-hour stirring at 500 rpm for 2 hours. After the reaction, the internal temperature of the reactor was lowered to 120 ° C, and stirring was continued at 500 rpm for 30 minutes. After the reaction, the remaining acetic anhydride was vaporized and removed first. Thereafter, in order to remove the remaining acetanhydride in the reactor secondarily, a step of neutralizing the acetianhyde hydrate by adding a 5% sodium chloride solution was performed. After the neutralization process, distilled water was added thereto, followed by washing with stirring, followed by phase separation, and finally, acetyltriethyl citrate was obtained. The composition of the product formed by the reaction was analyzed with a capillary column (HP-1, 50 m) and a gas chromatograph (GC: Younglin Co.) equipped with an FID detector. The analytical conditions are as follows: the temperature of the detector and the injector is 250 ° C,The temperature of the column was increased from 100 ° C to 250 ° C at a rate of 10 ° C / min and then maintained at this temperature for 20 minutes.

References:

Sunchon National University Industry-Academic Cooperation Foundation;Jeong Sang-cheol KR101793939, 2017, B1 Location in patent:Paragraph 0044-0048; 0079

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