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Process for preparing sodium stibogluconate

A technology of sodium antimony gluconate and sodium gluconate, which is applied in the field of chemical synthesis, can solve the problems of high production cost, low total yield, and high total consumption, and achieve the effects of reduced production cost and easy quality standards

Inactive Publication Date: 2005-07-06
王绍胜
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The total yield of the process technology for this production of sodium stibogluconate is low, only 60-70% (in terms of input sodium gluconate), methyl alcohol CH 3 The total amount of OH is high, which is 70 times the input amount of sodium gluconate, and the production cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Production method: Add 60 kg of water into the reaction tank, then put in 40 kg of sodium gluconate, stir and dissolve, add 40 kg of antimony trichloride, control the internal temperature at 35°C, add 60% sodium hydroxide until the pH is 9.8 , the dropwise addition is completed, keep warm and stir for 30 minutes, then lower the inner temperature to 26°C, add hydrogen peroxide dropwise to PH 6.0, stir for 30 minutes, add 3 kg of methanol, and filter to obtain sodium antimony gluconate solution after passing the test. The solution was added to 20 times methanol, crystallized, filtered and washed with methanol to chloride ion CL - Qualified, dried at 85°C to obtain 41.1 kg of sodium antimony gluconate.

Embodiment 2

[0016] Production method: Add 55 kg of water to the reaction tank, then put in 40 kg of sodium gluconate, stir and dissolve, add 40.08 kg of antimony trichloride, control the internal temperature at 37°C, add 60% sodium hydroxide until the pH is 9.6 , the dropwise addition is completed, keep warm and stir for 36 minutes, then lower the inner temperature to 28°C, add hydrogen peroxide dropwise to PH 5.7, stir for 30 minutes, add 2 kg of methanol, and filter to obtain sodium antimony gluconate solution after passing the test. The solution was added to 20 times methanol, crystallized, filtered and washed with methanol to chloride ion CL - Qualified, dried at 85°C to obtain 42.3 kg of sodium antimony gluconate.

Embodiment 3

[0018] Production method: Add 50 kg of water into the reaction tank, then put in 40 kg of sodium gluconate, stir and dissolve, add 40.03 kg of antimony trichloride, control the internal temperature at 40°C, add 40% sodium hydroxide until the pH is 9.5 , after the dropwise addition, keep stirring for 30 minutes, then lower the inner temperature to 26°C, add hydrogen peroxide dropwise to PH 5.5, stir for 30 minutes, add 4 kg of methanol, and filter to obtain sodium antimony gluconate solution after passing the test. The solution was added to 15 times methanol, crystallized, filtered and washed with methanol to chloride ion CL - Qualified, dried at 85°C to obtain 40 kg of sodium antimony gluconate.

[0019] Laboratory items

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Abstract

A process for preparing sodium stibogluconate is characterized by adding water in the reaction pot, adding sodium gluconate, mixing, adding antimonous chloride after dissolving, keeping the temperature of 28C.-48C., adding sodium hydroxide with the concentration of between 40 % and 60% to pH between 9.3 and 11.3, keeping the temperature and stirring for 20 to 40 Mins, then lowering the inner temperature to between 20C. and 36C., drop adding sodium hydroxide to pH between 4.6 and 6.0, and stirring for 20 to 40 Mins, adding methanol, after testing, filtering to getting the sodium stibogluconate solution, adding methanol to the solution, crystallizing, centrifuging and washing the chloride ion to get the demand by using methanol, and drying at the temperature of 60C. to 90C..

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, in particular to a new production process of sodium antimony gluconate. Background technique [0002] Sodium antimony gluconate is an intermediate raw material for pharmaceutical production. The technology provided by U.S. Patent No. 3,306,921 in 1967 is the first to use antimony trichloride SbCl 3 (82kg) dissolved in methanol CH 3 In OH (3.6L), dissolve sodium gluconate G-OONa (7.4kg) in water (18.5L), dissolve sodium hydroxide NaOH (4.0kg) in water (10L), then add in sequence, and finally When adding sodium hydroxide NaOH, immediately heat the solution to 90-95°C, after the reaction is completed and filtered, add methanol CH 3 OH (200L), a precipitate was formed, filtered, and washed with methanol CH 3 After washing with OH and drying, the obtained crude sodium antimony gluconate was dissolved in water (ratio 1:0.9), and the pH was adjusted to 6.3-6.4 with sodium hydroxide NaOH, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/41C07C59/105
Inventor 王绍胜
Owner 王绍胜
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