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A kind of preparation method of d-tryptophan

A tryptophan and white technology, applied in the field of D-tryptophan, can solve the problems of poor quality of D-tryptophan and high purity of D-tryptophan, and achieve low environmental pollution, high purity, simple and efficient process Effect

Active Publication Date: 2017-04-26
MAANSHAN DEHONG BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the deficiency of the poor quality of D-tryptophan in the prior art, a kind of D-tryptophan is provided, adopt the technical proposal of the present invention, its product D-tryptophan has high purity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] A kind of D-tryptophan of the present embodiment, its synthetic steps are:

[0047] Step A, first put L-tryptophan and solvent into the reaction kettle, then put in the racemic agent, raise the temperature to 40°C, stir for 0.5h, then add the resolving agent, and raise the temperature to 2°C / min at the same time 95°C, keep warm for 24 hours, wherein: the mass ratio of L-tryptophan to solvent is 1:4.8, the mass ratio of L-tryptophan to racemic agent is 1:0.39, the mass ratio of L-tryptophan to resolving agent The mass ratio is 1:0.9, the solvent in this example is water, the resolving agent is 2,3-dihydroxysuccinic acid, and the racemic agent is sodium hydroxide;

[0048] After step B, step A, carry out following temperature control process to the mixture that step A makes:

[0049] 1) Cool down to 90°C, keep warm for 24 hours,

[0050] 2) Cool down to 85°C, keep warm for 12h,

[0051] 3) Cool down to 80°C, keep warm for 10h,

[0052] 4) Cool down to 75°C, keep warm ...

Embodiment 2

[0073] A kind of D-tryptophan of the present embodiment, its synthetic steps are:

[0074] Step A, first put L-tryptophan and solvent into the reaction kettle, then put in the racemic agent, raise the temperature to 40°C, stir for 0.5h, then add the resolving agent, and raise the temperature to 2°C / min at the same time 95°C, keep warm for 24 hours, wherein: the mass ratio of L-tryptophan to solvent is 1:4.5, the mass ratio of L-tryptophan to racemic agent is 1:0.4, the mass ratio of L-tryptophan to resolving agent The mass ratio is 1:0.8, the solvent in this embodiment is water, the resolving agent is α-methylbenzylamine, and the racemic agent is salicylaldehyde;

[0075] After step B, step A, carry out following temperature control process to the mixture that step A makes:

[0076] 1) Cool down to 90°C, keep warm for 24 hours,

[0077] 2) Cool down to 85°C, keep warm for 12h,

[0078] 3) Cool down to 80°C, keep warm for 10h,

[0079] 4) Cool down to 75°C, keep warm for 15...

Embodiment 3

[0093] A kind of D-tryptophan of the present embodiment, its synthetic steps are:

[0094] Step A, first put L-tryptophan and solvent into the reaction kettle, then put in the racemic agent, raise the temperature to 40°C, stir for 0.5h, then add the resolving agent, and raise the temperature to 2°C / min at the same time 95°C, keep warm for 24 hours, wherein: the mass ratio of L-tryptophan to solvent is 1:5, the mass ratio of L-tryptophan to racemic agent is 1:0.38, the mass ratio of L-tryptophan to resolving agent The mass ratio is 1:1, the solvent in the present embodiment is water, the resolving agent is dextroamino, and the racemic agent is acetic acid;

[0095] After step B, step A, carry out following temperature control process to the mixture that step A makes:

[0096] 1) Cool down to 90°C, keep warm for 24 hours,

[0097] 2) Cool down to 85°C, keep warm for 12h,

[0098] 3) Cool down to 80°C, keep warm for 10h,

[0099] 4) Cool down to 75°C, keep warm for 15h,

[0...

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Abstract

The invention discloses D-tryptophan, which belongs to the technical field of D-tryptophan. The D-tryptophan has the following natures: (1) the D-tryptophan is white crystalline powder; (2) the chiral purity of the D-tryptophan reaches 100 percent; (3) the mass percentage of the D-tryptophan is more than 99.5 percent, and the light transmittance reaches more than 95 percent; (4) the HPLC (high performance liquid chromatography) detection content of the D-tryptophan can reach more than 99.5 percent; and (5) the density of the D-tryptophan is 1.232g / cm<2>, the smelting point is 282 to 285 DEG C, the boiling point is 399.4 DEG C at 760mmHg, the flashing point is 195.4 DEG C, and the water solubility at 20DEG C is 11g / L. The D-tryptophan is high in purity and pure in color, can reach the content of the medicine grade field, the needed product can be obtained through one-step reaction in the production process, and the complexity of the traditional process can be avoided.

Description

technical field [0001] The present invention relates to the technical field of D-tryptophan, more specifically, relates to a kind of D-tryptophan which can reach the content of pharmaceutical grade field. Background technique [0002] As a non-protein optically active amino acid, D-tryptophan has special physiological properties and has certain value in food, feed industry and agriculture. It can be used as non-nutritive sweetener, feed additive and plant growth agent. Especially in the pharmaceutical industry, D-tryptophan is an important synthetic precursor for anticancer agents and immunosuppressants. [0003] In the prior art, the preparation methods of D-tryptophan mainly include resolution method and biological method. Among them, the resolution methods include: 1) Membrane resolution method, which can be used to separate and process a large number of racemates due to the advantages of quickness, convenience, low relative energy loss and continuous operation; 2) Enzym...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D209/20
Inventor 祁超史凌云邢益胜杨建平
Owner MAANSHAN DEHONG BIOTECH