- Apr 27, 2018 -
The acetic acid, isopropyl alcohol and concentrated sulfuric acid were added to the enamel kettle, and the mixture was heated under reflux for more than 10 hours under stirring. After the temperature was lowered, the solution was neutralized to a pH of 7 to 8 with a saturated solution of sodium bicarbonate or sodium carbonate, washed with a saturated saline solution, and washed with water. Set the water layer, dry it with anhydrous sodium sulphate or magnesium sulfate, filter it, add it to the rectification tower for distillation, and collect the 85~95°C fraction, which is the finished product.
Purification method: often contains impurities such as water, acetic acid, and isopropyl alcohol. In the purification, 50 g of potassium carbonate was added to 100 mL of the ester and shaken well to remove the acid. The alcohol was further washed with a concentrated calcium chloride solution, and dried over anhydrous calcium chloride for 1 day and then distilled.