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A kind of preparation method of high-purity rocuronium bromide

A rocuronium bromide and high-purity technology is applied in the field of preparation of high-purity rocuronium bromide raw materials for non-depolarizing muscle relaxants, and can solve the problem that workshop safety has high requirements, conventional workshops are not suitable for industrialized operations, and The residual solvent of rocuronium bromide raw material cannot fully meet the requirements and other problems, and achieves the effects of low cost, high stability and simple process

Active Publication Date: 2021-02-02
江苏盈科生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of autoclaves as crystallization equipment is currently not suitable for industrial operations in conventional workshops, and has high requirements for workshop safety.
[0007] In US2006 / 0058275, isobutyl acetate and diethyl ether are used as anti-solvents to carry out crystallization in acetonitrile, but the residual solvent of the prepared rocuronium bromide raw material cannot fully meet the requirements, and needs to be processed in other ways

Method used

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  • A kind of preparation method of high-purity rocuronium bromide

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Effect test

Embodiment 1

[0036] The preparation of rocuronium bromide crude product:

[0037] Referring to Example 3 of patent US2006 / 0058275, the raw material (2β, 3α, 5α, 16β, 17β)-2-(4-morpholino)-16-(1-pyrrolyl)-androsta-3,17-di Alcohol-17-acetate (1200g) and 3-bromopropene (3600ml) were added to 5000ml of acetonitrile, stirred and reacted at room temperature for 3 hours, the reaction solution was slowly added to 30000ml of vigorously stirred ether, and the precipitated Roku Filtrate with ammonium bromide and dry overnight in vacuum to obtain crude rocuronium bromide.

[0038] The preparation of rocuronium bromide finished product:

[0039] Step 1) Dissolve 1.1 kg of rocuronium bromide crude product in 3 liters of 10% acetone aqueous solution, filter, and concentrate under reduced pressure to obtain a foamy solid ①;

[0040] Step 2) Add 0.9 kg of foamy solid ① and 4.4 kg of n-heptane into the homogenizer, after homogeneous dispersion, filter under nitrogen protection to obtain solid ②;

[0041]...

Embodiment 2

[0044] The preparation of rocuronium bromide crude product:

[0045] Referring to Example 2 of patent US2006 / 0058275, the raw material (2β, 3α, 5α, 16β, 17β)-2-(4-morpholino)-16-(1-pyrrolyl)-androsta-3,17-di Alcohol-17-acetate (120g) and 3-bromopropene (320ml) were added to 480ml of acetonitrile, stirred and reacted at room temperature for 3 hours, the reaction solution was slowly added to 2880ml of vigorously stirred ethyl acetate, and the precipitated Rocuronium bromide was filtered and vacuum dried overnight to obtain crude rocuronium bromide.

[0046] The preparation of rocuronium bromide finished product:

[0047] Step 1) rocuronium bromide crude product 100g is dissolved in the 12% acetone aqueous solution of 300ml, filters, and concentrates under reduced pressure, obtains foamy solid ①;

[0048] Step 2) Add 90 g of foamy solid ① and 540 g of n-heptane into a homogenizer, after homogeneous dispersion, filter under nitrogen protection to obtain solid ②;

[0049] Step 3...

Embodiment 3

[0052] The preparation of rocuronium bromide crude product:

[0053] The raw material (2β,3α,5α,16β,17β)-2-(4-morpholino)-16-(1-pyrrolyl)-androst-3,17-diol-17-acetate (120g ), 3-bromopropene (320ml) was added to 1000ml of dichloromethane, stirred and reacted at room temperature for 15 hours, the reaction solution was slowly added to 4000ml of vigorously stirred methyl tert-butyl ether, and the separated out rocuronium bromide Filter and dry overnight in vacuum to obtain crude rocuronium bromide.

[0054] The preparation of rocuronium bromide finished product:

[0055] Step 1) rocuronium bromide crude product 100g is dissolved in the 15% acetone aqueous solution of 300ml, filters, and concentrates under reduced pressure, obtains foamy solid ①;

[0056] Step 2) Add 90 g of foamy solid ① and 450 g of n-hexane into a homogenizer, and after homogeneous dispersion, filter under nitrogen protection to obtain solid ②;

[0057] Step 3) Add 90 g of n-hexane to 90 g of solid ②, stir a...

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Abstract

The invention provides a preparation method of high-purity rocuronium bromide, which comprises the steps of dissolving crude rocuronium bromide in aqueous acetone, filtering, concentrating under reduced pressure, adding n-heptane for homogenization, beating and the like. The preparation method of the high-purity rocuronium bromide provided by the invention has many advantages such as extremely low solvent residue, extremely high HPLC purity, extremely low content of related substances, and high stability.

Description

technical field [0001] The invention relates to the field of chemical pharmacy, in particular to a method for preparing a high-purity rocuronium bromide bulk drug of a non-depolarizing muscle relaxant. Background technique [0002] The chemical name of Rocuronium bromide is 1-[17β-acetoxy-3α-hydroxy-2β-(4-morpholinyl)-androstane-16β-yl]-1-(2-propene Base) pyrrole bromide, its chemical structural formula is as follows. [0003] [0004] Rocuronium bromide is a non-depolarizing muscle relaxant, which is commonly used clinically for endotracheal intubation, and can also be used to maintain muscle relaxation in various operations. After intravenous injection of rocuronium bromide, the onset of action is fast, and intubation can be performed within 60 to 90 seconds, and the action time lasts for 30 to 40 minutes. Rocuronium bromide has no significant effect on autonomic nerves and cardiovascular, but can reduce intraocular pressure, without histamine release and sympathetic ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J43/00
CPCC07J43/003
Inventor 李海陈文
Owner 江苏盈科生物制药有限公司
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