Method for judging reaction endpoint of diacetyl guanine and controlling quality of finished product

A technology of diacetylguanine and reaction end point, applied in the direction of comprehensive factory control, measuring device, color/spectral characteristic measurement, etc., can solve the problem of no effective method for reaction end point control and finished product quality control, difficulty in end point control and finished product quality, purine Problems such as insoluble ring structure

Active Publication Date: 2020-11-03
HUBEI HONGYUAN PHARMA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Diacetylguanine is an important intermediate of many nucleotide analog raw materials such as acyclovir, ganciclovir, valacyclovir hydrochloride, etc. The synthesis method using guanine as the starting material has been published, but the reaction end point There has been no effective method for control and quality control of finished products. Because of its extremely unstable properties, it can be deacylated rapidly in water, methanol, ethanol and other systems to form monoacetylguanine and guanine, and its purine ring structure is difficult in most organic solvents. It is difficult to control the end point control and finished product quality by conventional methods such as liquid, and often needs to further synthesize the next step product to evaluate its quality, which poses a huge risk to the production and process optimization of the product, and also causes drastic fluctuations in the quality of downstream products

Method used

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  • Method for judging reaction endpoint of diacetyl guanine and controlling quality of finished product
  • Method for judging reaction endpoint of diacetyl guanine and controlling quality of finished product
  • Method for judging reaction endpoint of diacetyl guanine and controlling quality of finished product

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Embodiment 1

[0023] A method for diacetylguanine reaction endpoint judgment and finished product quality control, comprising the following steps:

[0024] Step (1): Using guanine as a starting material, using a mixture of acetic anhydride and acetic acid as an acylating reagent and solvent, under the action of a catalyst, heat up to 129 degrees, after 18 hours of acylation reaction, take a small amount of reaction solution, and cool down to 20- 50°C, filter to obtain diacetylguanine filter cake, wash with a small amount of acetic acid or acetic anhydride, and filter dry to obtain batches of diacetylguanine wet product 2005008 and 2005009.

[0025] Step (2): use DMSO to prepare the 0.2-0.7 absorbance clarification solution allowed by UV spectrophotometry, detect the absorbance value at 307nm and 270nm with a UV spectrophotometer, or carry out 250-350 band scanning, calculate two kinds of wavelengths (wave peak and trough) absorbance ratio

[0026] Step (3): Use the same method to detect th...

Embodiment 2

[0030] Step (1): Using guanine as the starting material, using acetic anhydride and acetic acid mixture as the acylating reagent and solvent, the next batch of medium-quality diacetylguanine samples, and another batch of guanine control (Zhongjian Hospital), self-made monoacetylguanine control (purity greater than 99%).

[0031]

[0032] Step (2): Prepare the experimental solution (double sample) with the following concentration with DMSO:

[0033] Step (3): Dilute the above solution with DMSO until the absorbance of the solution is between 0.2-0.7, scan at 250-350nm, calculate the ratio of peak 306 to trough 273nm, and obtain the working curve, see Figure 8 and Figure 9 :

[0034] Available: guanine 0, 1%, 2%, 3%, 4%, 5% experimental diacetylguanine sample solution ultraviolet detection 306 / 273nm absorbance ratio (dual sample detection balance is good).

[0035] Diacetylguanine sample solutions containing 0, 1%, 2%, 3%, 4%, and 5% of monoacetylguanine were detected by...

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Abstract

The invention belongs to the technical field of quality control in a diacetyl guanine production process, and particularly relates to an efficient and convenient method for judging a reaction endpointof diacetyl guanine and controlling the quality of a finished product, which comprises the following steps: by taking guanine as an initial raw material and an acetic anhydride and acetic acid mixture as an acylation reagent and a solvent, performing heating to 120-140 DEG C under the action of a catalyst; performing reacting to generate diacetyl guanine, taking a proper amount of diacetyl guanine sample (reaction liquid needs to be pretreated), preparing an absorbance clarified solution within a proper range of ultraviolet spectrophotometry by using an aprotic solvent, detecting absorbance values at two positions by using an ultraviolet spectrophotometer, and calculating an absorbance ratio under two wavelengths. Compared with qualified diacetyl guanine, according to the discovery that the absorbance of a reaction solution is subjected to red shift in the process of generating diacetyl guanine through guanine reaction, the ultraviolet dual-wavelength absorbance ratio detection methodis adopted to compare qualified finished products, so that the reaction endpoint and the quality of the finished products can be quickly and accurately controlled.

Description

technical field [0001] The invention belongs to the technical field of quality control in the production process of diacetylguanine, and in particular relates to a method for judging the end point of diacetylguanine reaction and controlling the quality of finished products. Background technique [0002] Diacetylguanine is an important intermediate of many nucleotide analog raw materials such as acyclovir, ganciclovir, valacyclovir hydrochloride, etc. The synthesis method using guanine as the starting material has been published, but the reaction end point There has been no effective method for control and quality control of finished products. Because of its extremely unstable properties, it can be deacylated rapidly in water, methanol, ethanol and other systems to form monoacetylguanine and guanine, and its purine ring structure is difficult in most organic solvents. It is difficult to control the end point control and finished product quality by liquid and other conventiona...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/31G01N21/33
CPCG01N21/314G01N21/33G01N2021/3148Y02P90/02
Inventor 徐诚李晓晖杨明高汪宏福
Owner HUBEI HONGYUAN PHARMA
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