A kind of synthetic method of 4-methyl-5-ethoxyoxazole continuous saponification decarboxylation

A technology of ethoxyoxazole and ethyl ethoxyoxazole, applied in the field of compound synthesis, can solve the problems of low yield of 4-methyl-5-ethoxyoxazole, long reaction time and the like, and achieves The effect of avoiding prolonged contact, improving the reaction yield and shortening the reaction time

Active Publication Date: 2022-07-26
XIAMEN KINGDOMWAY VI TAMIN INC +1
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Problems solved by technology

[0007] The purpose of the present invention is to provide a method that can significantly increase the yield and shorten the reaction time in order to overcome the low yield and long reaction time defects when adopting the existing method to synthesize 4-methyl-5-ethoxy oxazole. Time continuous saponification decarboxylation method for synthesizing 4-methyl-5-ethoxy oxazole

Method used

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  • A kind of synthetic method of 4-methyl-5-ethoxyoxazole continuous saponification decarboxylation

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preparation example Construction

[0032] The synthetic method of 4-methyl-5-ethoxyoxazole continuous saponification decarboxylation provided by the invention comprises:

[0033] S1, the organic solution containing 4-methyl-5-ethoxyethyl oxazolate is continuously pumped into tubular reactor I after premixing with alkali to carry out saponification reaction to obtain saponification solution;

[0034] S2. After the saponification liquid is premixed with acid and alcohol, it is continuously pumped into tubular reactor II for decarboxylation reaction, the obtained decarboxylation liquid is discharged from the outlet of tubular reactor II, and 4-methyl-5- Ethoxyxazole.

[0035] There is no particular limitation on the specific types of the tubular reactor I and the tubular reactor II in the present invention, which can be various existing tubular reactors that can realize continuous synthesis and reduce back-mixing of reactants. Preferably, each independently is (50 to 200):1. Specifically, the tubular reactor I a...

Embodiment 1

[0046] S1, configure the 4-methyl-5-ethoxy oxazole acid ethyl ester toluene solution of 1mol / L respectively and the sodium hydroxide aqueous solution of 20%w / w, these two materials are 1 according to the volume ratio per unit time: After the ratio of 0.25 was fully mixed by the mixer and preheated to 50°C, it was sent to the tubular reactor I (straight-tube reactor) for reaction, the temperature of the reactor was controlled to be 60°C, and the residence time was 5 minutes to obtain a saponified solution. ;

[0047] S2, fully mix the saponification solution with concentrated hydrochloric acid (concentration is 36%~38%, the same below) and ethanol in a ratio of 1:0.12:0.25 according to the volume ratio per unit time and preheat to 60°C, then feed into the pipe Type reactor II (straight-tube reactor) reaction, control the temperature of the reactor to be 65 ℃, the residence time is 10 minutes, the decarboxylation liquid is discharged from the outlet of the tubular reactor II, an...

Embodiment 2

[0049] Synthesize 4-methyl-5-ethoxyoxazole according to the method of Example 1, the difference is that the organic solvent for dissolving ethyl 4-methyl-5-ethoxyoxazole is replaced with chloroform, The preheating temperature of the tubular reactor II was changed to 50°C, the decarboxylation reaction temperature was changed to 55°C, and the decarboxylation residence time was changed to 20 minutes, the same as in Example 1, to obtain 4-methyl-5-ethoxyoxazole, Its content was 99.10%, and the yield was 97.83%.

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Abstract

The invention belongs to the field of compound synthesis, and discloses a method for synthesizing 4-methyl-5-ethoxyoxazole continuous saponification and decarboxylation. The organic solution is premixed with alkali and then continuously pumped into tubular reactor I for saponification reaction. The obtained saponification solution is premixed with acid and alcohol and then continuously pumped into tubular reactor II for decarboxylation reaction. The outlet of the device II is discharged, and the 4-methyl-5-ethoxyoxazole is obtained after post-processing. The invention adopts the tubular reactor to carry out the continuous saponification and decarboxylation reaction, which can not only significantly shorten the reaction time and improve the reaction yield, but also reduce the steps of water stripping and distillation. process, reducing energy consumption.

Description

technical field [0001] The invention belongs to the field of compound synthesis, and in particular relates to a synthesis method for continuous saponification and decarboxylation of 4-methyl-5-ethoxyoxazole. Background technique [0002] 4-Methyl-5-ethoxyoxazole (II) is an intermediate of vitamin B6, which is generally obtained by saponification and decarboxylation of ethyl 4-methyl-5-ethoxyoxazole (I). The specific chemical The equation looks like this: [0003] [0004] The saponification and decarboxylation of traditional 4-methyl-5-ethoxy oxazole acid ethyl ester adopts batch process, and the concrete process is as follows: in the organic solution of 4-methyl-5-ethoxy oxazole acid ethyl ester Add sodium hydroxide aqueous solution, heat up to carry out saponification reaction, after the reaction is completed, let stand for stratification, add hydrochloric acid to the water layer to pH 1.5, then heat to carry out decarboxylation reaction, and then the obtained contains...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D263/42
CPCC07D263/42
Inventor 赵家宇苏珍莹詹欣马瑞达林兴
Owner XIAMEN KINGDOMWAY VI TAMIN INC
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