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A kind of preparation method of rocuronium bromide

A technology for rocuronium bromide and a compound, which is applied in the field of substance synthesis, can solve the problems of low yield, excessive residual impurities and solvent, easily excessive hydrolyzed impurities, etc., achieves good effect of removing solvent and residual, simplifies the difficulty of subsequent processing, The effect of high safety

Active Publication Date: 2021-04-30
武汉华龙生物制药有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In this process, rocuronium bromide is directly dissolved in water without any medium for protection, and its hydrolyzed impurity C is easy to exceed the standard
[0006] In summary, in the existing preparation method of rocuronium bromide, there are also technical problems that the yield is not high, and it is easy to cause impurities and solvent residues to exceed the standard and wait to be solved.

Method used

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  • A kind of preparation method of rocuronium bromide
  • A kind of preparation method of rocuronium bromide
  • A kind of preparation method of rocuronium bromide

Examples

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Embodiment 1

[0037] Embodiment 1 of the present invention provides a kind of preparation method of rocuronium bromide, comprises the steps:

[0038](1) Preparation of Compound III

[0039] Pump 72kg of dichloromethane into the reaction kettle at 25°C-30°C, start stirring, add 1.6kg of starting materials, stir and disperse; add 0.63kg of acetyl chloride dropwise, after dropping, keep the temperature of the material liquid at 25°C-30°C and stir React for 5 to 8 hours, the reaction solution is not processed, directly dropwise add 4.1kg of 10% hydrochloric acid solution to the reaction solution, after the drop is complete, keep the reaction at 25°C to 30°C for 20 hours, let stand and separate, remove 46.7kg of the organic layer, Add about 20.6 kg of 10% sodium carbonate aqueous solution to the remaining reaction solution to adjust pH=7 to 9, separate the organic phase, add 3.8 kg of silica gel to the organic phase, stir and absorb for 10 min, filter under reduced pressure, and then use 32.3 kg...

Embodiment 2

[0044] In this embodiment, except step 3 is changed to "the mass ratio of dichloromethane to methyl tert-butyl ether-ethyl acetate in the dichloromethane-methyl tert-butyl ether-ethyl acetate system is 8:20:20" , all the other are with embodiment 1.

Embodiment 3

[0046] In this embodiment, except that step 3 is changed to "the mass ratio of dichloromethane to methyl tert-butyl ether-ethyl acetate in the dichloromethane-methyl tert-butyl ether-ethyl acetate system is 3:25:25" , all the other are with embodiment 1.

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Abstract

The invention provides a preparation method of rocuronium bromide, comprising: step 1, reacting raw material compound I with acetyl chloride to prepare compound II; step 2, adding hydrochloric acid solution dropwise to compound II obtained in step 1 for hydrolysis reaction , standing for stratification, removing part of the organic layer, adjusting the pH of the remaining reaction solution to 7-9 with aqueous sodium carbonate solution, separating the organic phase and treating it to obtain compound III; step 3, compound III and allyl bromide, adding dichloro Methane, anhydrous magnesium sulfate, and basic aluminum oxide are subjected to quaternization reaction under nitrogen flow. After the reaction is completed, they are filtered under nitrogen protection. The pure product of rocuronium bromide is obtained after the system is beaten and solidified and freeze-dried; the purity of the prepared bulk drug product is ≥ 99.8% (result after correction according to USP40), the maximum impurity ≤ 0.1% (result after correction according to USP40), and the sum of solvent residues ≤0.5%.

Description

technical field [0001] The invention relates to the technical field of substance synthesis, in particular to a preparation method of rocuronium bromide. Background technique [0002] The chemical name of Rocuronium Bromide is 1-[(2β, 3α, 5α, 16β, 17β)-17-(acetyloxy)-3-hydroxy-2-(4-morpholinyl)androster- 16-yl]-1-propenylpyrrole ammonium bromide, its preparation trade name: Esmeron, the specification is 25mg / 2.5ml and 50mg / 5ml. It was the Dutch company Organon that first went public in the US and the UK in June and July 1994. Rocuronium bromide is an adjuvant drug for general anesthesia and is used for tracheal intubation during routine induction of anesthesia to maintain intraoperative skeletal muscle relaxation. Rocuronium bromide is a relatively new non-depolarizing steroidal muscle relaxant, which is characterized by rapid onset of action and no accumulation in the body. It has weak inhibitory effect on the cardiovascular system; has little effect on liver and kidney f...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J43/00
CPCC07J43/003
Inventor 丁冠军肖刚黄楚华郑丹伟别康伟殷婷
Owner 武汉华龙生物制药有限公司
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