Synthesis method of tert-butyl acetoacetate

Abstract

The invention discloses a synthesis method of tert-butyl acetoacetate. The method comprises the following steps that tertiary butanol and catalysts are added into a reaction container; the catalysts are selected from aliphatic amine catalysts or tertiary amine catalysts; or the catalysts are fatty amine catalysts and tertiary amine catalysts; the catalysts are one kind of catalysts or several kinds of catalysts proportioned at any proportion; the temperature is raised to 20 to 120 DEG C; diketene is dropwise added; in the reaction process, the reaction temperature is controlled to be 20 to 150DEG C; after the dripping is completed, the temperature is controlled at 20 to 150 DEG C; heat insulation is performed for 0.5 to 8 hours to obtain tert-butyl acetoacetate raw ester; the mole ratio of the tertiary butanol to the diketene is (1 to 2) to1; the addition of the catalyst is 0.1 weight percent to 2 weight percent of the total amount. The process is used for synthesizing the tert-butylacetoacetate; the conversion rate of the diketene reaches 100 percent; the finished product yield reaches 94 percent or higher; the product content reaches 99 percent or higher. By using the process,the synthesis yield is greatly improved; the preparation cost is reduced; meanwhile, the three-waste quantity is reduced; no corrosion is caused on the equipment; better economic and environment-friendly effects can be achieved.

Description

technical field [0001] The invention relates to the technical field of synthesis of tert-butyl acetoacetate, and relates to a new synthesis process of tert-butyl acetoacetate. Background technique [0002] tert-butyl acetoacetate [0003] Alias: tert-butyl 3-butanone; tert-butyl acetoacetate; [0004] English name: tert-Butyl acetoacetate [0005] Appearance properties: colorless, odorless and transparent liquid. [0006] Solubility: slightly soluble in water, soluble in xylene; [0007] CAS No.: 1694-31-1 [0008] [0009] Molecular weight: 158.195 [0010] Melting point (°C): -38 [0011] Boiling point (°C): 190 [0012] Relative density (water=1): 0.97 [0013] Flash point (℃): 76 [0014] Function and use: [0015] It is used as the raw material of medicine, pesticide and pigment, as the intermediate of organic synthesis, and mainly used as acetoacetylating agent. In the paint industry, the non-catalyst method used in the manufacture of acetoacetylated poly...

AI Technical Summary

Problems solved by technology

This route needs to use expensive metal sodium, the synthesis yield is low, and there is no mature industrialization report;

[0019] 3) It adopts diketene and tert-butyl alcohol to carry out the esterification reaction. The highest yield reported in the literature is 87%, the yield is low, the quality is poor, and the by-product tert-butyl ether is produced in the reaction process, which has a greater impact on the reaction yield.

[0020] All of the above processes have either expensive raw materials, low yields, or acid corrosion to the equipment, all of which lead to high production costs.

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