Reaction treatment method of heliotropin intermediate 3,4-dioxymethylene mandelic acid

Abstract

The invention discloses a reaction treatment method of heliotropin intermediate 3,4- dioxymethylene mandelic acid. The method comprises the following reaction treatment steps: firstly, adding glyoxylic acid in a reaction kettle, adding 1,3-benzodioxole under stirring action, and cooling the glyoxylic acid and 1,3-benzodioxole mixed liquid with brine ice; adding a catalyst, namely concentrated sulfuric acid; then dripping a water-insoluble inert solvent, namely dichloromethane, into a head tank, carrying sampling detection on a reaction mixture, and stopping reaction when the content of 1,3-benzodioxole in the reaction mixture is not reduced any more; and finally, adding water into the reaction kettle, uniformly stirring, discharging and filtering by suction to obtain the solid material, namely 3,4- dioxymethylene mandelic acid. According to the reaction treatment method, the feeding sequence is regulated in the early stage to improve the mixing effect and increase the reaction speed, and the water-insoluble inert solvent is added to dilute the reaction mixture, so that the stirring effect is not influenced, the reaction time is shortened, and the problem of hard stirring in the late reaction stage can be solved.

Description

technical field [0001] The invention relates to a reaction treatment method of jasmonal intermediate 3,4-methylenedioxymandelic acid. Background technique [0002] Jasmonal is also known as piperonal, heliopine, heliopine, pepper formaldehyde, oxidized piperonal, etc. Its chemical name is 3,4-methylenedioxybenzaldehyde, and its English name is: piperonal, helitropine, 3,4 -methylenedioxybenzaldehyde, molecular formula is C8H6O3, molecular weight is 150.13, wherein C accounts for 64.00%, H accounts for 4.03%, O accounts for 31.97%, its structure is as follows: [0003] [0004] The appearance of jasmonal is white shiny crystal, with a melting point of 37°C and a boiling point of 263°C; insoluble in water and glycerin, easily soluble in ethanol, ether, benzyl benzoate, diethyl phthalate, soluble in propylene glycol, in olive oil. Jasmonal is easy to change color under heat and light, and is stable in dilute acid and dilute alkali. [0005] Jasmonal is a very important in...

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Problems solved by technology

[0009] The present invention aims at the deficiencies of the prior art, and provides a reaction treatment method of jasmonal intermediate 3,4-methylenedioxymandelic acid with simple process, easy-to-obtain raw materials and mild reaction conditions, which solves the problem 3,4-methylenedioxymandelic acid synthesis reaction late stage stirring more and more difficult problem

This reaction treatment method adjusts the feeding order in the early stage to improve the mixing effect and speed up the reaction speed. In the secondary reaction, a water-insoluble inert solvent is added to dilute the reaction mixture to ensure that the stirring effect is not affected, which not only shortens the reaction time, Moreover, it solves the problem of difficult stirring in the later stage of the reaction, controls a constant reaction temperature, and avoids the generation of side reaction products.

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