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Preparation method of rocuronium bromide starting material (LK-7) single crystal

A technology of LK-7, rocuronium bromide, applied in the direction of single crystal growth, single crystal growth, chemical instruments and methods, etc.

Pending Publication Date: 2022-07-01
北京满格医药科技有限公司 +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There is no public report on the single crystal of LK-7 and rocuronium bromide

Method used

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  • Preparation method of rocuronium bromide starting material (LK-7) single crystal
  • Preparation method of rocuronium bromide starting material (LK-7) single crystal
  • Preparation method of rocuronium bromide starting material (LK-7) single crystal

Examples

Experimental program
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Embodiment 1

[0055] Example 1 LK-7 single crystal cultivation process:

[0056] About 0.3 g of LK-7 was added to a 20 ml vial, about 15 ml of dichloromethane was added, and the mixture was shaken to dissolve. Then add 5 drops of methanol and shake gently. Then add 1 to 2 drops of hydrochloric acid and shake it gently. Keep it still, cover it with a rubber stopper, insert a capillary tube on the rubber stopper to evaporate the solvent, place it at room temperature of about 25°C, keep it still, and observe it every other day. No crystals were seen on the second day of observation. On the fourth day, single crystals were found to be precipitated, and the single crystals were dispersed, with appropriate thickness and good shape.

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Abstract

The invention belongs to the technical field of raw material medicine preparation, and particularly relates to a single crystal culture method for a rocuronium bromide starting raw material (LK-7). According to the technical scheme, the method comprises the following steps: firstly, dissolving a certain amount of LK-7 solid in a proper amount of organic solvent at a certain temperature to obtain an LK-7 solution with a certain concentration, and meanwhile, ensuring that the obtained solution is clear and transparent without any macroscopic particles; and culturing the LK-7 single crystal by adopting a volatile solvent method. The invention provides a culture method of an LK-7 single crystal, and provides a scientific method for quality control of an initial bulk drug LK-7, especially for confirmation of an absolute configuration of a chiral center.

Description

technical field [0001] The invention belongs to the technical field of preparation of raw materials, and in particular relates to a preparation method of LK-7 single crystal. Background technique [0002] The chemical name of LK-7 is 2β-(4-morpholinyl)-16β-(1-pyrrolyl)-5α-androsta-3α,17β-diol. Its structure is as follows: [0003] [0004] LK-7 is a white to off-white powder, which is the starting material for the synthesis of rocuronium bromide. Rocuronium bromide is a white to slightly yellow powder. It is a steroid non-depolarizing muscle relaxant developed by Organon in the Netherlands. It was first marketed in the United States in 1994. Rocuronium bromide is a nondepolarizing neuromuscular blocking agent that is structurally similar to vecuronium and pancuronium. Like other non-depolarizing drugs, it competitively binds to cholinergic receptors on motor nerve terminal synapses to antagonize the effects of acetylcholine. The depolarizing neuromuscular blocking age...

Claims

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Application Information

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IPC IPC(8): C07J43/00C30B7/06C30B29/54
CPCC07J43/003C30B7/06C30B29/54C07B2200/13C07B2200/07
Inventor 汪澄申丹丹佘东来汪娟王晓红
Owner 北京满格医药科技有限公司
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