Preparation method of rocuronium bromide intermediate 5alpha-sterane-2-ene-17-one

A technology of rocuronide and an intermediate, which is applied in the field of pharmaceutical synthesis, can solve the problems of many by-products in the preparation process, cumbersome post-processing and high manufacturing cost, and achieves the effects of reducing energy consumption, shortening reaction time and reducing production cost.

Inactive Publication Date: 2020-03-24
ZENJI RES LAB
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Purpose of the invention: the purpose of the present invention is to provide a preparation method of rocuronium bromide intermediate 5α-stan-2-en-17-one, which solves the problem of too many by-products in the existing preparation process, cumbersome post-processing, and high manufacturing cost. high problem

Method used

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  • Preparation method of rocuronium bromide intermediate 5alpha-sterane-2-ene-17-one
  • Preparation method of rocuronium bromide intermediate 5alpha-sterane-2-ene-17-one
  • Preparation method of rocuronium bromide intermediate 5alpha-sterane-2-ene-17-one

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Experimental program
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Effect test

Embodiment 1

[0022] Add 140 grams (0.314 mol) of epiandrosterone TS, 210 grams of N,N-dimethylformamide, and 203 grams (0.628 mol) of tetrabutylammonium bromide into the reaction flask, start stirring and raise the temperature to 98 ° C for 23 hours After the reaction, the temperature was lowered to 55°C, water was added, solids were precipitated, filtered, the collected solids were stirred with water and then filtered again, the collected solids were dried to obtain 84.8 grams of 5α-stan-2-en-17-one.

Embodiment 2

[0024] Add 140 grams of epiandrosterone TS (0.314 mol), 280 grams of N,N-dimethylformamide, and 250 grams (0.785 mol) of tetrabutylammonium bromide into the reaction flask, start stirring and raise the temperature to 102°C for 24 hours After the reaction, the temperature was lowered to 60°C, water was added, solids were precipitated, filtered, the collected solids were stirred with water and then filtered again, the collected solids were dried to obtain 82.3 grams of 5α-stan-2-en-17-one.

Embodiment 3

[0026] Add 140 grams (0.314 mol) of epiandrosterone TS, 280 grams of N,N-dimethylformamide, and 220 grams (0.682 mol) of tetrabutylammonium chloride into the reaction bottle, start stirring and raise the temperature to 100 ° C for 23 hours After the reaction, the temperature was lowered to 58°C, water was added, solids were precipitated, filtered, the collected solids were stirred with water and then filtered again, the collected solids were dried to obtain 77.9 grams of 5α-stan-2-en-17-one.

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Abstract

The invention discloses a preparation method of a rocuronium bromide intermediate 5alpha-sterane-2-ene-17-one. The specific steps include: sequentially adding epiandrosterone TS, a solvent and a phasetransfer catalyst into a reaction bottle, performing heating to a reaction temperature of 90-120DEG C, carrying out stirring reaction, and conducting post-treatment purification to obtain the 5alpha-sterane-2-ene-17-one. The method provided by the invention greatly shortens the reaction time, reduces byproducts, enhances the yield, reduces three wastes, lowers the production cost, is suitable forindustrial production, and has obvious social and economic benefits.

Description

technical field [0001] The invention relates to the technical field of drug synthesis, in particular to a preparation method of rocuronium bromide intermediate 5α-stan-2-en-17-one. Background technique [0002] Rocuronium bromide (rocuronium bromide) is a non-depolarizing sterol muscle relaxant developed by Organon in the Netherlands. It was first launched in the United States in June 1994. It is the most effective non-depolarizing sterol muscle relaxant so far. The fast kind. It binds to the acetylcholine receptor through a competitive mechanism, prevents the activation of the acetylcholine channel and the depolarization of the cell membrane, and achieves the effect of muscle relaxation. This product has no histamine release, fast onset, good controllability, and small accumulation effect. It is mainly manifested by muscle relaxants and rapid induction of muscle relaxation of endotracheal intubation, and its structural formula is as follows: [0003] [0004] It has be...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07J1/00
CPCC07J1/0011
Inventor 葛敏李令超付明伟
Owner ZENJI RES LAB
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