A kind of penehyclidine hydrochloride impurity and preparation method thereof

A kind of penehyclidine and impurity technology is applied in the field of penehyclidine hydrochloride impurity and preparation thereof, can solve the problems such as no literature report in the compound preparation method, and achieves the effects of low cost, good economic value and strong practicability

Active Publication Date: 2022-06-28
NHWA PHARMA CORPORATION
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The compound and its preparation method have not been reported in the literature at present

Method used

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  • A kind of penehyclidine hydrochloride impurity and preparation method thereof
  • A kind of penehyclidine hydrochloride impurity and preparation method thereof
  • A kind of penehyclidine hydrochloride impurity and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Penehyclidine base preparation:

[0038] In a 250ml beaker, add 20g penehyclidine hydrochloride, 50ml 10% NaOH solution, 100ml ethyl acetate and stir to clarify, let stand for separation, the aqueous phase is extracted twice with ethyl acetate (200ml / time), the organic phases are combined and saturated Washed with brine, dried over anhydrous magnesium sulfate, and concentrated to dryness to give a colorless oil.

Embodiment 2

[0039] Embodiment 2: the preparation method of compound shown in formula I

[0040] All the oily substances prepared in Example 1, 300 ml of THF were added to the 500 reaction flask, stirred to dissolve, 15.7 g of m-chloroperoxybenzoic acid was added in batches, the addition was completed, and the mixture was stirred at room temperature for 36 hours.

[0041] 200ml of saturated sodium carbonate solution was added to the reaction solution, adjusted to pH 8-9, left to stand for layers, the aqueous phase was extracted twice with tetrahydrofuran (200ml / time), the organic phases were combined, dried over anhydrous magnesium sulfate, and concentrated to dryness. 15.3 g of yellow oil was obtained.

[0042] The crude product was dissolved in 100 ml of tetrahydrofuran, 15.3 g of neutral aluminum oxide (200-300 mesh) was added, and concentrated to dryness under reduced pressure, and the sample was used for later use. In addition, 153g of neutral aluminum oxide (200-300 mesh) was added ...

Embodiment 3

[0045] The preparation method of compound shown in embodiment 3 formula I

[0046] (1) All the oils prepared in Example 1 and 300 ml of THF were added to 500 reaction flasks, stirred to dissolve, 15.7 g of m-chloroperoxybenzoic acid was added in batches, and the mixture was stirred at room temperature for 28 hours.

[0047](2) 200ml of saturated sodium carbonate solution was added to the reaction solution, adjusted to pH 8-9, left to stand for stratification, the aqueous phase was extracted twice with tetrahydrofuran (200ml / time), the organic phases were combined and dried over anhydrous magnesium sulfate , concentrated to dryness to obtain 16.0g of yellow oil.

[0048] (3) Dissolve the crude product with 100 ml of tetrahydrofuran, add 32 g of neutral aluminum oxide (200-300 mesh), concentrate to dryness under reduced pressure, and use the sample for later use. In addition, 320g of neutral aluminum oxide (200-300 mesh) was added to 2L of ethyl acetate. After stirring evenly, ...

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Abstract

The invention relates to a penhyclidine hydrochloride impurity and a preparation method thereof, belonging to the technical field of medicine. The penehyclidine impurity provided by the present invention is shown in formula I, and the impurity reference substance 3-(2-cyclopentyl-2-hydroxyl-2-phenylethoxy) quinine-1-oxide synthesis method provided , the synthetic raw materials are easy to obtain, the operation is simple and convenient, the cost is low, and it has good economic value.

Description

technical field [0001] The invention relates to a penehyclidine hydrochloride impurity and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Penehyclidine hydrochloride is an anticholinergic drug with a new structure of M receptor antagonists, chemical name: 3-(2-cyclopentyl-2-hydroxy-2-phenylethoxy) quinuclidine salt acid salt, the structural formula is as follows: [0003] [0004] In the prior art, penehyclidine hydrochloride is not only used for the first aid treatment of organophosphorus poisoning (pesticide) poisoning, the maintenance of atropine in the later stage of poisoning or after cholinesterase (ChE) aging, but also for pre-anesthetic administration. It is used clinically to inhibit the secretion of salivary glands and airway glands, and has a wide range of applications. According to various preclinical studies, penehyclidine hydrochloride also has strong safety, mainly in that it has no potential toxi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D453/02
CPCC07D453/02
Inventor 王勇张稳王圣庆许向阳
Owner NHWA PHARMA CORPORATION
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