Preparation method of alkyl furanone

Abstract

The invention relates to a preparation method of alkyl furanone. The preparation steps are as follows: dripping acetyl tert-butyl acetate into absolute aether containing sodium metal until aether reflow, maintaining reflux after finishing dripping to obtain mixed solution A; dripping alpha-bromo-propionyl chloride into mixed solution A at 12-15 DEG C, maintaining the temperature after finishing dripping, standing at room temperature, precipitating the organic phase and washing with water, extracting the aqueous layer with aether, merging the organic phase and drying to obtain mixed solution B; evaporating mixed solution B out of aether, carrying out reduced pressure reaction on the residual liquid to obtain mixed solution C; and refining mixed solution C, blending with water, regulating pH value with sodium hydroxide solution to 7.9-8, adding hydrogen peroxide, regulating pH value of the product with hydrochloric acid solution to 1-2, extracting with aether, drying extract, removing aether and carrying out reduced pressure evaporation to obtain pale yellow oil-solid mixture, i.e. finished product of alkyl furanone. The preparation method has short technique period, simple operation, satisfactory yield, and good color, scent and flavor of the finished product.

Description

technical field [0001] The invention belongs to the field of organic compounds, in particular to a preparation method of alkyl furanone. Background technique [0002] Alkyl furanone is a widely used food spice, which has a strong sauce and fruity aroma, and occupies an important position in the flavoring industry. 4-hydroxy-2,5-dimethyl-3(2H)-furanone (4-Hydroxy-2,5-dimethyl-3(2H)-Furanone, hereinafter referred to as HDMF) in alkyl furanone spices, because of its strong The sauce aroma and pineapple aroma are more representative. HDMF can be used not only as a spice, but also as an intermediate and combined with a sulfide heterocyclic compound to transform into a substance that can emit various aromas. There are many existing methods for synthesizing HDMF, but there are certain disadvantages, such as: (1). The further cyclization of 3-ethylene-2,5-diol can be used to oxidize ozone to obtain HDMF. (2). Utilize crotonoyl nitrile and ethyl lactate to prepare HDMF chlorination...

AI Technical Summary

Problems solved by technology

There are many existing methods for synthesizing HDMF, but there are certain disadvantages, such as: (1). The further cyclization of 3-ethylene-2,5-diol can be used to oxidize ozone to obtain HDMF. (2). Utilize crotonoyl nitrile and ethyl lactate to prepare HDMF chlorinated condensation method under alkaline condition, still exist the deficiency of low yield; (3). Also can utilize α-alkyl- Diethyl diglycolic acid and diethyl monoacid are condensed to prepare HDMF. Although the yield of this method is high, the raw materials are highly toxic, and the process is complicated and the cycle is long.