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Glycyl-L-glutamine preparation method

A technology of glutamine and glycyl, which is applied in the field of preparation of glycyl-L-glutamine, can solve the problems of ammonium salt easily blocking the condenser, inconvenient production, long concentration time and the like, and achieves short concentration time, The effect of not easy to remove and short reaction time

Active Publication Date: 2014-04-02
JINAN CHENGHUI SHUANGDA CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The introduction of a large amount of ammonium salt requires secondary concentration (add 2025ml of water after concentration to dryness, and continue to concentrate), and nearly 11.14 times of water needs to be evaporated. The concentration time is long, because the ammonium salt needs to be taken out by steam, and the ammonium salt is cooled when the condenser is cooled. Easy to block the condenser, not convenient for production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (a) Preparation of crude glycyl-L-glutamine

[0027] In the plastic-lined high-pressure reactor, add 100kg of chloroacetyl-L-glutamine to dissolve it in 500kg of water, feed ammonia gas to 0.2~0.4Mpa, slowly raise the temperature to 42°C, at 42±1°C, 0.2~0.4 Stir under Mpa pressure for 5 hours; concentrate under reduced pressure, after 30 minutes, the temperature rises to 55~65°C, the vacuum is not higher than -0.09Mpa, concentrate until nearly dry, add 120kg of water, stir, heat to 52~56°C, add 2kg of activated carbon, Keep stirring for 25 minutes, filter out activated carbon, add 250kg methanol, keep stirring for 30 minutes, cool down to -4~-1°C, cool down and crystallize for 2~2.5 hours, centrifuge, and dry at 40~50°C for 8~10 hours to obtain off-white solid 82.8 kg, the liquid phase purity is not less than 97.8%;

[0028] (b) Glycyl-L-glutamine refining

[0029] Dissolve 82.5kg of crude product in 165kg of water, heat to 52~56℃, add 1.65kg of activated carbon,...

Embodiment 2

[0031] (a) Preparation of crude glycyl-L-glutamine

[0032] In the enamel reaction kettle, dissolve 200kg of chloroacetyl-L-glutamine in 1000kg of water, feed ammonia gas to 0.2~0.4Mpa, slowly raise the temperature to 42°C, and stir for 5 hours at 45°C under a pressure of 0.2~0.4Mpa; Concentrate under reduced pressure, after 30 minutes, the temperature rises to 55~65°C, the vacuum is not higher than -0.09Mpa, concentrate to nearly dry, add 240kg of water, stir, heat to 52~56°C, add 4kg of activated carbon, keep stirring for 25min, filter out the activated carbon , add 500kg of methanol, heat and stir for 30min, cool down to -4~-1°C, cool down and crystallize for 2~2.5 hours, shake off the material, dry at 40~50°C for 8~10 hours, and obtain 165.9kg of off-white solid. Less than 98.1%.

[0033] (b) Glycyl-L-glutamine refining

[0034] Dissolve 165kg of crude product in 330kg of water, heat to 52~56℃, add 3.3kg of activated carbon, keep stirring for 25min, filter out the activa...

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Abstract

The invention belongs to the technical field of drug synthesis and particularly relates to a glycyl-L-glutamine preparation method. According to the glycyl-L-glutamine preparation method provided by the invention, a crude product of the glycyl-L-glutamine is prepared by introducing ammonia gas into the glycyl-L-glutamine and conducting ammonolysis under pressure, and then refining is conducted to obtain a pure product of the glycyl-L-glutamine. The glycyl-L-glutamine is taken as the raw material and is dissolved with water whose amount is 5 times that of the raw material, the ammonia gas is introduced, the ammonolysis is conducted under pressure, the reaction time is only 5h and is short, no ammonium salt is introduced in the reaction process, the volume of a solvent to be evaporated is small, the concentration time is short, and the preparation method is convenient to operate and is suitable for industrial production. The purity of the prepared glycyl-L-glutamine is not less than 99.3%.

Description

technical field [0001] The invention belongs to the technical field of medicine synthesis, and in particular relates to a preparation method of glycyl-L-glutamine. Background technique [0002] Glycyl-L-glutamine, formula C 7 h 13 N 3 o 4 ·H 2 O, molecular weight 221.21, structural formula [0003] . [0004] Glycyl-L-glutamine is an amino acid drug and one of the main active ingredients of compound amino acid (15) dipeptide (2) injection. [0005] In the patent CN1532204A, the glycine amino group is used for protection, and then, it is made into an active ester, and then docked with L-glutamine, and finally, the protecting group is removed by palladium carbon reduction. This method has long steps and cumbersome operation, and is not suitable for industrialized production. And patent CN1740188A takes glutamic acid as starting material, first forms ester, and uses light bulb bottle to place one week during ammonolysis, and this method cycle is longer, and equipment...

Claims

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Application Information

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IPC IPC(8): C07K5/062C07K1/22C07K1/02
Inventor 王庭见王素兰刘速凌王倩
Owner JINAN CHENGHUI SHUANGDA CHEM
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