4-methoxy methyl acetoacetate preparation method
2015
The invention discloses a 4-methoxy methyl acetoacetate preparation method. The 4-methoxy methyl acetoacetate preparation method comprises the following steps of adding a solvent tetrahydrofuran into a reaction kettle and leading inert gas into the reaction kettle, setting the internal temperature of the reaction kettle to be 15 DEG C to 25 DEG C, adding industrial sodium hydride and a metal alkaline compound in a stirring state, then adding the solvent tetrahydrofuran, dropwise adding mixed liquid of methyl alcohol and methyl-4-chloroacetoacetate at the temperature of lower than 20 DEG C to perform reaction for 4-6 hours, rising the temperature to be 20 DEG C to 25 DEG C to continue to react for 4-15 hours, reducing the system temperature to be 6 DEG C to 10 DEG C after TLC detection reaction is completed, adding a hydrochloric acid solution with molar concentration of 2 mol/L to regulate the pH of a system to be 5 to 7, performing standing and laying, concentrating and spin-drying upper-layer liquid to remove the solvent tetrahydrofuran after liquid separation and then obtaining a colorless product 4-methoxy methyl acetoacetate through wiped-film molecular distillation. The 4-methoxy methyl acetoacetate can react at room temperature, a product can be produced at low temperature through distillation, and dangerousness in the production process and product impurity content can be directly and effectively reduced.
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