The preparation method of 4-methyl-5-alkoxy oxazole

A technology of alkoxy oxazole and methyl, which is applied in the field of preparation of 4-methyl-5-alkoxy oxazole, can solve the problems of unfavorable industrial production, long reaction steps, and the need for catalysts, and achieve low scrap rate , low equipment requirements, high selectivity and conversion

Active Publication Date: 2021-01-05
SHANDONG NHU FINE CHEM SCI & TECH CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many side reactions, many impurities, low yield, low selectivity, a stoichiometric catalyst is required, and the reaction steps are long, which is not conducive to industrial production

Method used

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  • The preparation method of 4-methyl-5-alkoxy oxazole
  • The preparation method of 4-methyl-5-alkoxy oxazole
  • The preparation method of 4-methyl-5-alkoxy oxazole

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preparation example Construction

[0050] The present invention provides a kind of preparation method of 4-methyl-5-alkoxy oxazole, it is characterized in that, described method comprises: carry out cyclization reaction with the compound shown in following formula (I) structure, with Obtaining said 4-methyl-5-alkoxyoxazole,

[0051]

[0052] Wherein, R represents the alkyl group of C1~C6;

[0053] The cyclization reaction is carried out in the presence of a solid acid catalyst.

[0054]

[0055]In the preparation method of 4-methyl-5-alkoxy oxazole in the present invention, the starting reactant used is the compound of formula (I), that is, N-formyl alanate. The starting reactant can be a single kind of N-formylalanine ester or a mixed starting reactant of multiple kinds of N-formylalanine esters, and the compound of formula (I) is cyclized by dehydration 4-Methyl-5-alkoxyoxazole is formed.

[0056] Wherein, the R in the formula (I) represents but not limited to the alkyl of C1~C6, can be straight-chain...

Embodiment 1

[0126] In a 1L three-necked flask, 145g (1mol) of ethyl N-formylalanine, 276g (3mol) of toluene and 20% CH(OSO 3 h) 3 / SiO 2 Solid acid (3.4g, 0.2mol%, active ingredient meter), start stirring device and stir, and be heated up to 90 ℃, after insulation reaction 10h, be lowered to room temperature, filter, obtain solid acid and reaction liquid respectively, the obtained solid The acid was directly put into the next batch of reactions without significant catalytic deactivation, wherein the conversion rate of the reaction was 93%, and the selectivity was 97.8%.

Embodiment 2

[0128] In a 1L three-necked flask, 131g (1mol) of N-formylalanine methyl ester, 276g (3mol) of toluene and 20% CH(OSO 3 h) 3 Solid acid (3.4g, 0.2mol%), turn on the stirring device to stir, and heat up to 80 ° C, after 10 hours of heat preservation reaction, cool down to room temperature, filter, respectively, to obtain solid acid and reaction solution, and directly put the obtained solid acid into the One batch was reacted without significant catalytic deactivation, wherein the conversion of the reaction was 80.3% and the selectivity was 90.4%.

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Abstract

Disclosed is a method for preparing 4-methyl-5-alkoxy oxazole, which belongs to the field of chemical synthesis. The method comprises subjecting a N-formylalaninate ester to a cyclization reaction to obtain the 4-methyl-5-alkoxy oxazole. The cyclization reaction is carried out in the presence of a solid acid catalyst. The purpose of the present invention is to provide a method for preparing 4-methyl-5-alkoxy oxazole having few reaction steps, a high yield, a low waste liquid discharge amount, easy pollution control, and low production costs. The method of the present invention can be applied to laboratory preparation or industrial production for the preparation of intermediates in the synthesis of vitamin B6.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, and in particular relates to a preparation method of 4-methyl-5-alkoxy oxazole. Background technique [0002] 4-Methyl-5-alkoxyoxazole, the specific structure is shown below, which is a synthetic vitamin B 6 important intermediate [0003] [0004] In the formula, R is a C1-C4 saturated alkyl group. [0005] Most of the synthetic methods of 4-methyl-5-alkoxy oxazole use N-alkoxy oxalyl alanine ester as raw material through dehydrating agent dehydration cyclization, then carry out saponification, decarboxylation, refining to the cyclization liquid obtained Distillation yielded the target product. [0006] Cited document 1 discloses a kind of industrial preparation method of 4-methyl-5-ethoxy oxazole, and specifically discloses and comprises the following steps: drop into N-ethoxy oxalyl alanamide in a certain proportion in the cyclization reactor Acetate ethyl ester, solid phosgene, chloro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D263/42C07D213/66
CPCC07D213/66C07D263/42
Inventor 林波王玉岗陈卫勇邵闪梁昊赵雷王海涛盛美兰吴元元杨小春
Owner SHANDONG NHU FINE CHEM SCI & TECH CO LTD
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