Preparation of ethyl acetate experiment

Summary

This experiment is from the official website of Jimei University

Operation method

Preparation of ethyl acetate experiment

Move

Apparatus:

Heating jacket; 250 mL triple-necked flask; 75° elbow; straight condenser tube; vacuum pick-up tube; 150 mL conical flask; vacuum stopper; 125 mL dropping funnel (19# for all of the above); thermometers (200°C, 100°C); 2 500 mL beakers; volumetric cylinders (10mL, 100mL); 125 mL dispensing funnel; distillation head 19#.

Drugs:

95% ethanol; concentrated sulfuric acid; saturated sodium bicarbonate solution; saturated sodium chloride solution; saturated calcium chloride solution; anhydrous magnesium sulfate.

1. Synthesis

Add 9 mL of 95 % ethanol to a 100 mL dry three-necked flask 19#, immerse the flask in ice water into

cool, slowly add 12 mL of concentrated sulfuric acid and mix, add a mixture consisting of 14 mL of 95 % ethanol and 14.3 ml of glacial acetic acid to a dropping funnel, the end of the foot of the funnel with the thermometer's mercury bulb must be immersed in the liquid below the level of the liquid from the bottom of the flask for about 0.5 to 1 cm, add 2 grains of zeolite, the receiver is immersed in ice water for cooling, and the branch pipe connected to the tailpipe is connected to a rubber hose leading to the sewer.

First to the three-necked bottle to add 3-4mL of the mixture, and then the three-necked bottle with a heating jacket carefully heated to 110-120 ℃ or so, when the distillation port should be liquid out, and then from the dropping funnel to slowly add the rest of the mixture, the control of the drop acceleration rate and the distillation rate is roughly equal to the speed of the distillation (1d/s), to maintain the reaction temperature of 110 ~ 125 ℃, about 0.5 h drop is completed, and then continue to heat, until the temperature rises to 130 ℃ not in the distillate until, remove the heat source to stop the reaction.

2. Refinement

Neutralize with 10 mL of saturated sodium bicarbonate solution until no carbon dioxide gas escapes, the ester layer was washed with 10 mL of saturated NaCl solution, 10 mLx2 saturated CaCl2 solution. Anhydrous magnesium sulfate was dried for 0.5 h and distilled in a water bath to collect fractions with boiling points at 73~78 °C.

Caveat

1. Add concentrated sulfuric acid in batches, shaking and cooling while adding to prevent oxidation of ethanol.

2. The device should be tight, after the reaction to cease fire, slightly cooled before removing the receiver, to prevent the product volatilization.

3. Control the reaction temperature and the speed of adding ethanol 1d/s.

4. Pay attention to the order of washing, no open flame in the room.

5. Dry with anhydrous magnesium sulfate for about 20~30 minutes after splitting clean water.

6. Product acceptance volume and boiling point.

For more product details, please visit Aladdin Scientific website.

https://www.aladdinsci.com/