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ChemicalBook CAS DataBase List Diethyl adipate
141-28-6

Diethyl adipate synthesis

12synthesis methods
Diethyl adipate is synthesized by esterification of adipic acid and ethanol in the presence of concentrated sulfuric acid.
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Yield:141-28-6 95.7%

Reaction Conditions:

with zeoliteReagent/catalyst;

Steps:

1.1-1.5; 2-10; 1-8 Step 1.
Add 2 g of zeolite to a three-necked flask.At the same time, 30g Mg2+ loaded resin catalyst is loaded on the upper part of the tower.Then, 146 g of adipic acid and 365 g of ethanol accurately weighed by an electronic balance were added to a conical flask to form a mixed mass of a certain mass ratio.Pour into the tower kettle;Step 2, the tower top condenser cooling water switch and the tower kettle control power supply are set, the heating rate is set to 5 ° C / min, and the acid value before the reaction is determined by using the calibrated NaOH standard solution;Step 3: After the reflux occurs at the top of the tower, after 20 minutes of stabilization, the top constant pressure funnel starts to feed, and the reflux ratio control switch is turned on.The reflux ratio is controlled to 1, and the timing starts, and the reaction starts;Step 4. When the top of the column is fed, the reaction is over, and the reaction time is recorded. At this time, the tower pressure is increased.Distilling excess methanol in the reaction system to purify the product,When the temperature at the bottom of the tower rises to 110 ° C, stop heating and turn off the power;Step 5,After 2h,The retentate in the column was refluxed, and the three-barrel flask was cooled, and then distilled under reduced pressure at 4.0 Kpa.Collecting 148-152 ° C fraction to obtain liquid diethyl adipate;

References:

Xuzhou Shunping Biological Technology Co., Ltd.;Zhao Ke;Sun Xin CN109704969, 2019, A Location in patent:Paragraph 0007; 0008; 0009-0025

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