Semi-synthesis method for high-purity and high-stability gastrodin

A high-stability, gastrodin technology, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problem that acetyl gastrodin cannot be directly separated, the stability of acetyl gastrodin is not good, and the cost of production management is increased. and other problems, to achieve the effect of low price, improved yield and reduced production cost

Active Publication Date: 2014-05-21
KPC PHARM INC
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Problems solved by technology

However, Raney nickel or palladium charcoal has many disadvantages in the catalytic hydrogenation of catalysts: 1. The catalyst is expensive and the operations such as purchase and storage are troublesome. The recovery and reuse of the catalyst is also an extremely complicated matter, which brings difficulties for industrial continuous production. Pollution hazards caused by the surrounding environment; 2. Catalytic hydrogenation has special

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  • Semi-synthesis method for high-purity and high-stability gastrodin

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preparation example Construction

[0023] Such as figure 2 As shown, the semi-synthetic method of high-purity and high-stability gastrodin described in the present invention comprises the steps of preparing acetylgastrodin, crude gastrodin, refining gastrodin, and recovering crude gastrodin, specifically including:

[0024] A. Preparation of acetylgastrodin: use tetraacetyl as raw material, add alcohol solvent or alcohol ester mixed solvent with a volume-to-weight ratio of 2 to 50 times, control the system temperature ≤ 10°C, add a reducing agent for reduction reaction, stir until the reaction liquid Adding the chromogenic agent does not show red, that is, stop the reaction; add acid to adjust the pH to 2~8, concentrate the reaction solution to 1.5~6 times the volume-to-weight ratio of tetraacetyl, and then add 0~12 times the volume ratio to the concentrated solution The water is filtered and dried to obtain acetylgastrodin, and the filtrate is reclaimed as mother liquor a for recycling;

[0025] B. Crude gas...

Embodiment approach

[0029] A. Preparation of acetylgastrodin: use tetraacetyl as raw material, add alcohol solvent or alcohol ester mixed solvent with a volume-to-weight ratio of 3 to 25 times, control the system temperature at 0°C to 5°C, add a reducing agent for reduction reaction, and stir until Adding the color developer dropwise to the reaction liquid does not show red color, that is, stop the reaction; add acid to adjust the pH to 6~7, concentrate the reaction liquid to 1.5~6 times the volume-to-weight ratio of tetraacetyl, and then add a volume ratio of 4~6 to the concentrated solution. 6 times of water, filtered and dried to obtain acetylgastrodin with a yield of 92-98%; reclaim the filtrate as mother liquor a for recycling;

[0030] B. Crude gastrodin: Add methanol, ethanol or propanol with a volume-to-weight ratio of 2 to 10 times the volume to weight of the prepared acetyl gastrodin, add alkali to adjust and maintain the system pH ≥ 6, and stop the reaction after 0.5 to 3 hours of reflu...

Embodiment 1

[0044] Take 1 kg of tetraacetyl, add 5 L of methanol-methyl formate mixed solvent with a volume ratio of 3:1 and mix evenly; control the temperature of the system at 6°C, add potassium borohydride for reduction reaction, and continue stirring; after 28 minutes of reaction, take a sample and add dropwise color agent, the reaction stops when there is no color development (if the color is red, continue to add potassium borohydride for reaction); after the reaction is stopped, add perchloric acid, adjust the pH to 6, concentrate the volume of the reaction solution to 5L, and add to the concentrated solution Add 30L of water, stir evenly, filter and dry to obtain 0.96kg of acetylgastrodin, with a yield of 95.58%; the filtrate is mother liquor a, which is recovered for subsequent use;

[0045] Add 3L of methanol to 0.96kg of acetylgastrodin, feed ammonia gas to adjust and maintain the pH of the system to 7, stop the reaction after 2 hours of reflux reaction, concentrate to 1.5L, add ...

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Abstract

The invention discloses a semi-synthesis method for high-purity and high-stability gastrodin. The semi-synthesis method comprises the following steps: carrying out a reduction reaction by taking tetraacethyl as a raw material; concentrating and adding a suitable amount of water into concentrated liquid; filtering and drying to obtain acethyl gastrodin; recycling a filtering solution which is used as a mother solution a; adding an alcohol solvent into the acethyl gastrodin to carry out a reflowing reaction, and concentrating; repeatedly reflowing and concentrating to obtain a concentrated solution; adding a non-polar solvent and filtering; drying solids to obtain a gastrodin rough product; recycling a filtering solution which is used as a mother solution b; adding alcohol and/or an ester solvent into the rough product of gastrodin; heating and completely dissolving; filtering and separating out crystals to obtain a refined product of gastrodin; recycling a filtering solution which is used as a mother solution c; mixing the mother solution b and the mother solution c; filtering and drying to obtain the rough product of gastrodin; and refining to obtain the refined product of gastrodin. The acethyl gastrodin prepared by the semi-synthesis method disclosed by the invention is stable, can be directly used as a crude drug, and can also be used as an intermediate to synthesize the high-purity gastrodin; the semi-synthesis method for the high-purity and high-stability gastrodin is very good for meeting the clinical demands on gastrodin and acethyl gastrodin.

Description

technical field [0001] The invention belongs to the technical field of drug synthesis, and in particular relates to a semi-synthetic method of gastrodin with high purity and high stability. Background technique [0002] Gastrodin is a natural compound and the core active ingredient of Gastrodia elata. Gastrodin has various physiological activities such as sedative, hypnotic, and anticonvulsant, and is mainly used clinically to treat dizziness, headache, deafness, tinnitus, and neurasthenia. In the late 1970s, Zhou Jun and others isolated a new compound from the traditional Chinese medicine Gastrodia elata, which was identified as 4-hydroxymethylphenyl-β-D-glucopyranoside. Pharmacological studies showed that this compound has sedative properties. , Hypnotic effect, considered to be the active ingredient of the traditional Chinese medicine Gastrodia elata, named gastrodin. In 1980, Zhou Jun and others completed the chemical synthesis of gastrodin, and after the continuous re...

Claims

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Application Information

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IPC IPC(8): C07H15/203C07H1/00
Inventor 谢波孙刚张红峰海龙宇谢科顾静波
Owner KPC PHARM INC
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