Preparation method of ethyl acetoacetate
A technology of ethyl acetoacetate and ethanol, applied in the preparation of ketene/polyketene, organic chemistry, etc., can solve the problems of reduced product purity, high rectification requirements, difficult filtration, etc., and achieves reduced raw material consumption and improved rectification. Yield, the effect of simple process operation
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Embodiment 1
[0035] A kind of preparation technology of ethyl acetoacetate, comprises the following steps:
[0036] Preparation of amine-type ionic liquid catalyst: Add 15.4g (0.21mol) of n-butylamine into a three-necked flask, slowly add 12.0g (0.2mol) of glacial acetic acid dropwise, after the addition is complete, heat to 60°C and continue the reaction for 2 hours to obtain light yellow Liquid n-butylamine acetate with a yield of 95%.
[0037]Esterification process: Add 41.07g of ethanol and 0.082g of catalyst n-butylamine acetate ionic liquid into a 500ml three-necked flask, heat up and reflux, add 50g of diketene dropwise, after 2h, keep warm at 120°C for 3h, detect no diketene, and the reaction is over. After being rectified by a rectifying tower, the finished product of ethyl acetoacetate is distilled out to obtain 76.4g of ethyl acetoacetate, the product yield is 98.8%, and the product content is 99.72%
Embodiment 2
[0039] Add 41.07g of ethanol and 0.27g of n-butylamine acetate ionic liquid into a 500ml three-necked flask (refer to Example 1 for the preparation of n-butylamine acetate ionic liquid), raise the temperature to reflux, add 50g of diketene dropwise, and dropwise add 2h, at 120°C Insulate for 3 hours, detect no diketene, the reaction is over, and then distill out the finished product of ethyl acetoacetate after rectification in a rectification tower to obtain 75.9g of ethyl acetoacetate, the product yield is 98.1%, and the product content is 99.75%
Embodiment 3
[0041] Add 41.07g of ethanol and 0.46g of catalyst n-butylamine acetate ionic liquid into a 500ml three-necked flask (refer to Example 1 for the preparation of n-butylamine acetate ionic liquid), raise the temperature to reflux, add 50g of diketene dropwise, and dropwise add 2h, at 120°C Keep warm for 3 hours, detect that there is no diketene, and after the reaction is completed, the finished product of ethyl acetoacetate is distilled out after rectification in a rectification tower to obtain 76.3 g of ethyl acetoacetate, the product yield is 98.6%, and the product content is 99.8%.
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