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Method for preparing D-cysteine hydrochloride-hydrate

A technology of cysteine ​​hydrochloride and cystine hydrochloride is applied in the field of preparation of D-cysteine ​​hydrochloride monohydrate, which can solve the problem that the optical purity of the product cannot meet the requirements and the requirements of crystallization temperature Strict and difficult to select solvents, etc., to achieve the effects of easy control, less equipment investment, and easy production and operation

Inactive Publication Date: 2011-10-19
曹县思达化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the process is simple, the optical purity of the obtained product cannot meet the requirements because the solvent is not easy to select and the crystallization temperature is extremely strict. Repeated recrystallization is required, and the operation is more cumbersome.

Method used

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  • Method for preparing D-cysteine hydrochloride-hydrate
  • Method for preparing D-cysteine hydrochloride-hydrate
  • Method for preparing D-cysteine hydrochloride-hydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation method of D-cysteine ​​hydrochloride monohydrate adopts the following steps:

[0037] (1) 500 kilograms of acetone, 141 kilograms of L-cysteine ​​hydrochloride and 47 kilograms of sodium carbonate were successively dropped into a reaction kettle equipped with a thermometer and an agitator, stirred and heated, reflux reaction at 60° C. for 5 hours, and cooled to 10 Filtrate at ℃, and reserve the mother liquor;

[0038] (2) Add 100 kg of anhydrous acetic acid and 120 kg of L-tartaric acid to the mother liquor in step (1), heat up at 50°C-55°C to induce racemization for 7 hours, cool down at 15°C-20°C and suction filter to obtain the dextrorotatory intermediate , filtrate recovery;

[0039] (3) Put 700 kg of purified water and 200 kg of dextrorotatory intermediate into the reaction kettle equipped with a thermometer and agitator successively, start stirring, heat up to 50°C, keep stirring for 4 hours, then cool down to 20°C-25°C, 50 kg of aqueous hydrogen...

Embodiment 2

[0042] The preparation method of the D-cysteine ​​hydrochloride monohydrate adopts the following steps:

[0043] (1) Put 800 kilograms of acetone, 141 kilograms of L-cysteine ​​hydrochloride and 55 kilograms of sodium carbonate into a reaction kettle equipped with a thermometer and an agitator successively, stir and heat up, reflux reaction at 55° C. for 4 hours, and cool down to 15 Filtrate at ℃, and reserve the mother liquor;

[0044] (2) Add 100 kg of anhydrous acetic acid and 120 kg of L-tartaric acid to the mother liquor in step (1), heat up at 50°C-55°C to induce racemization for 7 hours, cool down at 15°C-20°C and suction filter to obtain the dextrorotatory intermediate , filtrate recovery;

[0045] (3) Put 700 kg of purified water and 200 kg of dextrorotatory intermediate into the reaction kettle equipped with a thermometer and agitator successively, start stirring, heat up to 50°C, keep stirring for 4 hours, then cool down to 20°C-25°C, 50 kg of aqueous hydrogen per...

Embodiment 3

[0048] The preparation method of the D-cysteine ​​hydrochloride monohydrate adopts the following steps:

[0049] (1) 500 kilograms of acetone, 141 kilograms of L-cysteine ​​hydrochloride and 47 kilograms of sodium carbonate were successively put into a reaction kettle equipped with a thermometer and an agitator, stirred and heated, refluxed at 60°C for 5 hours, and cooled to - Filter at 5°C and reserve the mother liquor;

[0050] (2) Add 150 kg of anhydrous acetic acid and 120 kg of L-tartaric acid to the mother liquor of step (1), heat up at 50°C-55°C to induce racemization for 5 hours, cool down at 15°C-20°C and suction filter to obtain the dextrorotatory intermediate , filtrate recovery;

[0051] (3) Put 700 kg of purified water and 200 kg of dextrorotatory intermediate into the reaction kettle equipped with a thermometer and agitator successively, start stirring, heat up to 50°C, keep stirring for 4 hours, then cool down to 20°C-25°C, 50 kg of aqueous hydrogen peroxide s...

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Abstract

The invention relates to a method for preparing a medicine intermediate, and particularly discloses a method for preparing D-cysteine hydrochloride-hydrate. The method for preparing the D-cysteine hydrochloride-hydrate is characterized by comprising the following steps of: carrying out neutralization cyclization on L-cysteine hydrochloride to obtain a ring-closing product; carrying out racemization on the ring-closing product, adding revulsive, transforming and separating out a dextral intermediate; carrying out hydrolysis ring-opening on the dextral intermediate, oxidizing to obtain D-cystine; and carrying out electrolysis concentration and crystallization on the D-cystine to obtain the D-cysteine hydrochloride-hydrate. By transforming the L-cysteine hydrochloride into the D-cysteine hydrochloride-hydrate, the method for preparing the D-cysteine hydrochloride-hydrate greatly lowers the production cost, the D-cysteine hydrochloride-hydrate has high yield and good quality, less emission of three wastes as an organic solvent is used as a reaction medium; and the production flow is simple, no high-temperature and high-pressure reaction exists, the equipment investment is less, and the production operation is easy.

Description

(1) Technical field [0001] The invention relates to a preparation method of a pharmaceutical intermediate, in particular to a preparation method of D-cysteine ​​hydrochloride monohydrate. (2) Background technology [0002] D-cysteine ​​hydrochloride is an important intermediate of the third-generation cephalosporin antibiotic drug - cefaminophen sodium. Cefaminophen sodium is a cephalomycin derivative, which is prepared by a semi-synthetic method. Its action properties are similar to those of the third-generation Cephalosporins are similar, and the finished product is heptahydrate, which has antibacterial effects on Escherichia coli, Streptococcus, Klebsiella, Haemophilus influenzae, Bacteroides, etc. hindrance. The lipoprotein structure is unique to Gram-negative bacteria, so its effect on Gram-negative bacteria is stronger than other similar drugs. At the same time, D-cysteine ​​hydrochloride is also a strong inhibitor of Escherichia coli and an effective reliever of acu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C323/58C07C319/02
Inventor 王平生刘志强崔平刚梁志红赵士杰
Owner 曹县思达化工有限公司
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