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A technology of triclotrione and trimethylbenzaldehyde, applied in the field of preparation of triclotrione, can solve the problems of low product yield, layered emulsification, complicated steps of triclotrione, etc., and achieves high product quality, The effect of increasing the reaction speed and avoiding by-products
Active Publication Date: 2021-06-25
SHENYANG SCIENCREAT CHEM
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Problems solved by technology
[0005] The technical problem to be solved by the present invention is that in the prior art, the steps of the preparation method of benzotrione are complicated, the product yield is low, and the washing after adding propionyl chloride in the process of synthesizing the second intermediate tends to cause more serious layered emulsification phenomenon. question
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preparation example Construction
[0049] figure 1 It is a process flow chart of the method for preparing trimethylbenzotrione according to the embodiment of the present invention. The preparation method of the embodiment of the present invention can be applied to the preparation of trimethylbenzotrione, and the preparation method is figure 1 each step in the .
[0050] figure 1 A kind of method for preparing trimethylbenzotrione provided by the present invention is shown, and described method comprises:
[0051] S1, using 2,4,6-trimethylbenzaldehyde and acetone to prepare the first intermediate;
[0052] S2, using the first intermediate, diethyl malonate and propionyl chloride to prepare the second intermediate;
[0053] S3, using the second intermediate and ethoxyamine to prepare trimethylbenzotrione;
[0054] In the process of preparing the second intermediate, condensation and rearrangement reactions are carried out simultaneously; after the preparation of the first intermediate and before the preparat...
example 1
[0088] This example adopts a one-pot method to prepare trimethylbenzotrione. It should be noted that the product obtained in the previous step does not need to be separated or purified in advance between the following steps.
[0089] 1. Synthesis of the first intermediate
[0090] The synthetic route of the first intermediate is:
[0091]
[0092] first intermediate
[0093] Table 1 first intermediate synthesis feed list
[0094]
[0095] Steps:
[0096] Put 2,4,6-trimethylbenzaldehyde, acetone, water, and sodium hydroxide solution into the four-necked bottle according to the actual dosage shown in Table 1, heat up to reflux under stirring, and keep the temperature within the range of 72-76°C Keep reflux for 4 hours; remove about 90mL of solvent under normal pressure, then cool down to below 70°C, add toluene, separate layers, reflux the toluene layer and divide water, then cool down to 25-30°C to obtain the toluene solution of the first intermediate.
[0097] 2. Syn...
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Abstract
The invention discloses a method for preparing tralkoxydim. The method comprises the following steps: preparing a first intermediate from 2,4,6-trimethylbenzaldehyde and acetone; preparing a second intermediate from the first intermediate, diethyl malonate and propionyl chloride; and preparing tralkoxydim by utilizing the second intermediate and ethoxyamine, wherein in the process of preparing the second intermediate, a condensation reaction and a rearrangement reaction are carried out at the same time, and after the first intermediate is prepared and before tralkoxydim is prepared, separation or purification treatment is not carried out. According to the invention, tralkoxydim is prepared by simultaneously carrying out condensation and rearrangement reactions and not carrying out a separation or purification process in the reaction process, so the steps of multiple times of separation, purification, transfer, feeding and the like in existing preparation methods are omitted, time and labor are saved, the consumption of reagents is reduced, a large amount of cost is saved, and the problems that a tralkoxydim preparation method is complex in step, product yield is low and layering emulsification is serious in an esterification reaction process in the prior art are solved.
Description
technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a preparation method of trimethylbenzotrione. Background technique [0002] Trimethylbenzotrione, the chemical formula is C 20 h 27 NO 3 , the structural formula is Belongs to oxime herbicides. [0003] At present, the method for preparing trimethylbenzalone is basically to condense 2,4,6-trimethylbenzaldehyde with acetone to obtain 1-(2,4,6-trimethylphenyl)-1-butene- 3-ketone, and then the product is separated and reacted with diethyl malonate and hydrolyzed, cyclized, and decarboxylated to obtain 3-hydroxy-5-(2,4,6-trimethylphenyl)-cyclohexyl-2 -en-1-one, the product is isolated again followed by reaction with propionic anhydride to give 3-hydroxy-5-(2,4,6-trimethylphenyl)-2-propionyl-cyclohex-2-ene-1 -ketone, and finally react with ethoxyamine hydrochloride to obtain trimethylbenzotrione. [0004] The above synthesis process generally needs to go through mu...
Claims
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