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 achieve reduced raw material consumption and simple process operation , Improve the effect of rectification yield
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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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