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Green and intelligent preparation method of high-purity diquafosol tetrasodium

A high-purity technology for tetrasodium phosphazene, which is applied in the field of green and intelligent preparation of high-purity diquafosor tetrasodium, can solve the problems of complicated process, high difficulty in operation, large loss and the like, and achieves simple and fast operation and complicated operation. , the effect of reducing energy consumption

Active Publication Date: 2020-09-15
NANJING CHENXIANG MEDICAL RES +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, the production of diquafosol tetrasodium at home and abroad adopts anhydrous reaction route. All raw materials, auxiliary materials, intermediates and equipment must be dehydrated. The reaction conditions are high, the process is cumbersome, the operation is difficult, and the product needs repeated recrystallization. Once, the crystallization has to be placed for a long time every time, which is time-consuming and troublesome, with great losses, and it is difficult to make it green and intelligent

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  • Green and intelligent preparation method of high-purity diquafosol tetrasodium

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preparation example Construction

[0047] The invention provides a method for preparing green and intelligent diquafosol tetrasodium, comprising the following steps:

[0048] 1) In the presence of the first condensing agent, condense disodium uridine monophosphate and disodium hydrogen phosphate dodecahydrate at 55°C to synthesize disodium uridine diphosphate;

[0049] 2) In the presence of the second condensing agent, uridine diphosphate disodium, magnesium chloride hydrate, and 4-dimethylaminopyridine are condensed again at 55° C. to generate diquafosol tetrasodium.

[0050] In the present invention, under the condition that the first condensing agent exists, uridine monophosphate disodium and dodecahydrate disodium hydrogen phosphate undergo condensation reaction at 55 DEG C to synthesize uridine diphosphate disodium.

[0051] In the present invention, the first condensing agent is preferably dissolved in an auxiliary agent; the auxiliary agent is preferably a water-acetonitrile mixed solution; the volume rati...

Embodiment 1

[0064] The preparation method of embodiment 1 diquafosol tetrasodium (batch production 50g)

[0065] 1. The preparation method of uridine diphosphate disodium (UDP 2Na)

[0066] Add 3 liters of 50% acetonitrile aqueous solution and 0.57 kg of 1,3-dimethyl-2-chloroimidazoline hexafluorophosphate (DMP) to the reaction flask that has been placed in cold water at 0°C, stir to dissolve, and control the temperature At 0°C, add 0.285kg imidazole (IM) and stir to dissolve, heat up to 40°C, stir and react for 10 minutes, add 0.25kg UMP·2Na (see the HPLC spectrum of uridine URD Figure 4 ; The HPLC collection of illustrative plates of uridine monophosphate disodium (UMP 2Na) reference substance sees Figure 5 ), stirred and reacted at 40°C for 30 minutes, then added 0.425kg of disodium hydrogen phosphate 12 hydrate, heated to 55°C, continued to stir and react for 4 hours, filtered, the filtrate was rotary evaporated to recover acetonitrile for reuse, and added pure water to the remaini...

Embodiment 2

[0070] The preparation of embodiment 2 diquafosol tetrasodium (batch production 500g)

[0071] 1. Synthesis of uridine diphosphate disodium (UDP·2Na)

[0072] Add 30 liters of 50% acetonitrile aqueous solution and 5.7 kg of 1,3-dimethyl-2-chloroimidazoline hexafluorophosphate (DMP) in sequence to the reactor placed in cold water at 0°C, stir to dissolve, and control the temperature At 0°C, add 2.85kg of imidazole (IM) and stir to dissolve, raise the temperature to 40°C, stir for 10 minutes, add 2.5kg of UMP·2Na, stir for 30 minutes at 40°C, then add 4.25kg of disodium hydrogen phosphate dodecahydrate , heat up to 60°C, continue to stir and react for 4 hours, filter, and recycle the filtrate to recover acetonitrile for use, add pure water to dilute the remaining liquid to 10g UMP / L liquid, pass through the HZ-201 resin column, first use 13BV 0.06N sodium chloride and Wash with a mixed solution of hydrochloric acid with a pH value of 2, then elute with a mixture of 11BV 0.12N s...

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Abstract

The invention provides a green and intelligent preparation method of high-purity diquafosol tetrasodium, and belongs to the technical field of chemical pharmacy. The green and intelligent diquafosol tetrasodium preparation method comprises the following steps: in the presence of a first group of condensing agent, condensing uridine disodium monophosphate and disodium hydrogen phosphate dodecahydrate at 55 DEG C to generate uridine disodium diphosphate; and in the presence of a second group of condensing agent, carrying out self-condensation on uridine disodium diphosphate, hydrated magnesium chloride and 4-dimethylaminopyridine again at 55 DEG C to generate diquafosol tetrasodium. The method provided by the invention has the advantages that the reaction is a water reaction, the main raw materials do not need to be subjected to sodium removal, all the raw materials, auxiliary materials, containers, reactors and the like do not need to be subjected to anhydrous treatment, the purification process is intelligently controlled, repeated long-time recrystallization is not needed, the operation is simple, energy is saved, emission is reduced, and the quality is stable and controllable.

Description

technical field [0001] The invention belongs to the technical field of chemical pharmacy, and in particular relates to a green and intelligent method for preparing high-purity diquafosol tetrasodium. Background technique [0002] Dry eye syndrome is a type of disease that causes eye discomfort and visual dysfunction due to tear film instability and / or ocular surface damage caused by abnormal tear volume or quality or fluid dynamics, also known as keratoconjunctival sicca. It is about 5.3% to 33.7% in the world, and about 21% to 30% in China. Women are more than men, and the elderly are more than young people. The incidence rate in China is higher than that in European and American countries. It is reported that the incidence rate in my country is about 45%. Among them, women are higher than men, and the elderly are higher than young people, which seriously affects the work and quality of life of patients. The lack of tears stimulates reflex tear secretion, which causes freque...

Claims

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Application Information

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IPC IPC(8): C07H19/10C07H1/06
CPCC07H19/10C07H1/06Y02P20/582
Inventor 邢为藩邢宸吴祖栋
Owner NANJING CHENXIANG MEDICAL RES
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