Preparation method and application of alpha-(o-chloroaniline) methylene-beta-formylaminopropionitrile

A technology of -formamidopropionitrile and o-chloroaniline, which is applied in the field of preparation of α-methine-β-formamidopropionitrile, can solve the pollution of the operating environment by turnover throwing, complicated operation requirements, and high labor intensity and other issues to achieve the effect of avoiding throwing waste, avoiding pollution of the operating environment, and reducing labor intensity

Pending Publication Date: 2022-03-25
江苏兄弟维生素有限公司
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  • Description
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AI Technical Summary

Problems solved by technology

However, using solid α-sodium formyl-β-formamidopropionitrile as a raw material, there are technical defects such as turnover polluting the operating environment, high labor intensity, long operating cycle, and complex operating requirements.

Method used

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  • Preparation method and application of alpha-(o-chloroaniline) methylene-beta-formylaminopropionitrile

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preparation example Construction

[0033] According to a first aspect of the present invention, a kind of preparation method of α-(o-chloroanilino) methine-β-formamidopropionitrile is provided, comprising the following steps:

[0034] The aqueous solution of α-sodioformyl-β-formamidopropionitrile reacts with the acid solution of o-chloroaniline to obtain α-(o-chloroaniline)methine-β-formamidopropionitrile.

[0035] In the present invention, the aqueous solution of α-sodium formyl-β-formamidopropionitrile is used to replace its solid as a raw material, which avoids the waste of solid materials in the turnover feeding process and the problem of polluting the operating environment, and also reduces The labor intensity of on-site operators is reduced, and since the aqueous solution of α-sodioformyl-β-formylaminopropionitrile is used, there is no need to control the solid α-sodioformyl-β-formyl simultaneously during the reaction process. The addition speed of aminopropionitrile and acid and the control of pH value g...

Embodiment 1

[0061] (a) adding 80g tap water, 76g o-chloroaniline and 105g of hydrochloric acid with a mass fraction of 25% to the reaction flask successively under stirring, and then continuing to stir for 10 minutes to obtain the hydrochloric acid solution of o-chloroaniline;

[0062] (b) 220g tap water is used to dissolve 100g of α-sodioformyl-β-formamidopropionitrile solid (its purity is 80%) to obtain an aqueous solution of α-sodioformyl-β-formamidopropionitrile;

[0063] (c) Add the α-sodioformyl-β-formamidopropionitrile aqueous solution of step (b) to the hydrochloric acid solution of o-chloroaniline in step (a) at a constant speed for about 5 minutes to obtain a reaction system;

[0064] (d) The reaction system of step (c) was incubated at a temperature of 40°C for 8 hours for condensation reaction, and then the product was centrifuged and filtered, and the product was washed with tap water until the pH was 7.0, and then dried to obtain the crude product α-(o-chloroaniline) 126.5 g...

Embodiment 2

[0066] (a) adding 100g tap water, 80g o-chloroaniline and 110g of hydrochloric acid with a mass fraction of 25% to the reaction flask successively under stirring, and then continuing to stir for 15 minutes to obtain the hydrochloric acid solution of o-chloroaniline;

[0067] (b) 250g tap water is used to dissolve 100g of α-sodioformyl-β-formamidopropionitrile solid (its purity is 80%) to obtain an aqueous solution of α-sodioformyl-β-formamidopropionitrile;

[0068] (c) Add the α-sodioformyl-β-formamidopropionitrile aqueous solution of step (b) to the o-chloroaniline hydrochloric acid solution of step (a) at a constant speed for about 10 minutes to obtain a reaction system;

[0069] (d) The reaction system of step (c) is kept at a temperature of 50° C. for 10 hours for condensation reaction, and then the product is centrifuged and filtered, and the product is washed with tap water until the pH is 7.0, and then dried to obtain the crude product α-(o-chloroaniline) 127 g of methi...

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Abstract

The invention provides a preparation method and application of alpha-(o-chloroaniline)-based methenyl-beta-formylaminopropionitrile, and relates to the technical field of chemical synthesis.The preparation method comprises the steps that an aqueous solution of alpha-sodium formyl-beta-formylaminopropionitrile and an acid solution of o-chloroaniline are subjected to a reaction, and alpha-(o-chloroaniline)-based methenyl-beta-formylaminopropionitrile and o-chloroaniline are subjected to a reaction to obtain alpha-(o-chloroaniline)-based methenyl-beta-formylaminopropionitrile; the alpha-(o-chloroaniline)-based methine-beta-formylamino propionitrile is obtained. The method solves the technical problems that solid alpha-sodium formyl-beta-formylaminopropionitrile is taken as a raw material in the traditional synthesis process, so that the operation environment is polluted by turnover throwing, the labor intensity is high, the operation period is long, the operation requirement is complex and the like; the technical effects of small operation environment pollution, simple operation, low labor intensity and short operation period are achieved.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a preparation method of α-(o-chloroanilino) methine-β-formamidopropionitrile and its application. Background technique [0002] Usually, the process for the synthesis of α-(o-chloroaniline) methine-β-formamidopropionitrile is to first add water, o-chloroaniline and hydrochloric acid of a certain concentration in a stirred state, then fully stir, and then Add solid α-sodium formyl-β-formamidopropionitrile into the reaction system within a certain period of time, and simultaneously add a certain concentration of hydrochloric acid to control the pH of the reaction system to 2.5-3. Insulation, after the reaction is completed, filter, wash with water and dry to obtain α-(o-chloroaniline) methine-β-formamidopropionitrile. However, the use of solid α-sodium formyl-β-formamidopropionitrile as a raw material has technical defects such as polluting the operating environment by ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C253/30C07C255/44C07C209/74C07C211/52C07D417/06
CPCC07C253/30C07C209/74C07D417/06C07C211/52C07C255/44
Inventor 严建斌王诚陈英明段艳文
Owner 江苏兄弟维生素有限公司
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