A kind of preparation method of dl-homosulfoalanine

A high sulfoalanine and homocystine technology, which is applied in the field of preparation of DL-homosulfoalanine, can solve the problem that the product purity cannot meet the requirements, the toxicity of DL-homosulfoalanine is high, Problems such as low product quality, to achieve the effects of pollution prevention, high quality, and clean preparation methods

Active Publication Date: 2018-10-09
CHONGQING TIANYI HENGHUA TECH CO LTD
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  • Claims
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Problems solved by technology

[0003] Aiming at the above-mentioned problems in the prior art, the present invention proposes a kind of preparation method of DL-homosulfoalanine, the present invention solves the problem that the process of preparing DL-homosulfoalanine in the prior art has high toxicity and poor product quality. High, the technical problem that the product purity can not meet the requirements

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  • A kind of preparation method of dl-homosulfoalanine

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Embodiment 1

[0017] A preparation method of DL-homosulfoalanine comprises: dissolving 268gDL-homocystine in 150g hydrochloric acid, heating up to 55°C for the first time, then adding 1862.5g sodium hypochlorite dropwise, after the dropwise addition, and then Raise the temperature twice to 75°C for 1.5 hours to obtain the reaction liquid; concentrate the reaction liquid obtained in step 1 to a small volume, then add an appropriate amount of ethanol to crystallize, then filter to obtain solid crystals, and then dry the crystals to obtain the target The product was 247gDL-homosulfoalanine, the yield was 67.5%, and the purity was 93.4%.

Embodiment 2

[0019] A kind of preparation method of DL-homosulfoalanine comprises: 268gDL-homocystine is dissolved in 200g hydrochloric acid, be warmed up to 60 ℃ for the first time, then dropwise add 2000g sodium hypochlorite, after dropwise addition, then second Raise the temperature to 80°C and react for 2 hours to obtain the reaction solution; concentrate the reaction solution obtained in step 1 to a small volume, then add an appropriate amount of ethanol to crystallize, then filter to obtain solid crystals, and then dry the crystals to obtain the target product 300gDL-homosulfoalanine, the yield is 82%, and the purity is 98.2%.

Embodiment 3

[0021] A preparation method of DL-homosulfoalanine comprises: dissolving 268gDL-homocystine in 250g hydrochloric acid, heating up to 65°C for the first time, then adding 2160.5g sodium hypochlorite dropwise, after the dropwise addition, then Raise the temperature to 85°C for 2.5 hours to obtain the reaction liquid; concentrate the reaction liquid obtained in step 1 to a small volume, then add an appropriate amount of ethanol to crystallize, then filter to obtain solid crystals, and then dry the crystals to obtain the target The product was 300gDL-homosulfoalanine, the yield was 82%, and the purity was 98.2%.

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Abstract

The present invention discloses a DL-homocysteic acid preparation method comprising the following steps: (1) dissolving DL-homocystine in an appropriate amount of hydrochloric acid, firstly heating to the temperature of 50 DEG C-70 DEG C, then adding dropwise sodium hypochlorite, after the addition is complete, then secondly heating to the temperature of 75 DEG C-85 DEG C for reaction for 1 to 3 hours to obtain a reaction solution; and (2) concentrating the reaction solution obtained in step (1) to a small volume, then adding an appropriate amount ethanol, crystallizing, then filtering to obtain a solid crystal, and drying thee solid crystal to obtain a DL-homocysteic acid desired product. The new method for preparation of the DL-homocysteic acid by reaction of the DL-homocystine and the sodium hypochlorite in the hydrochloric acid avoids use of bromine as a reactant, and avoids pollution generated by the use of bromine, and the DL-homocysteic acid product prepared by the method is high in quality and has the purity more than 98%.

Description

technical field [0001] The invention relates to a preparation method of DL-homosulfoalanine. Background technique [0002] DL-homosulfoalanine is an important intermediate in chemical synthesis and new pharmaceutical synthesis. The main method for preparing DL-homosulfoalanine is to dissolve DL-homocystine in hydrochloric acid. , then add bromine dropwise to react, after the reaction, concentrate the reaction solution to the minimum volume; then add an appropriate amount of ethanol to crystallize, then filter, and dry the filtered crystals to obtain the product DL-high sulfopropane Amino acid; reactant has used bromine in this reaction, and bromine toxicity is big, and pollution is also bigger; The product quality of the DL-homosulfoalanine prepared by this method is not high, and the purity of product is about 95% . Contents of the invention [0003] Aiming at the above-mentioned problems in the prior art, the present invention proposes a kind of preparation method of D...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C303/16C07C309/18
CPCC07C303/16C07C309/18
Inventor 郑伟唐勇
Owner CHONGQING TIANYI HENGHUA TECH CO LTD
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