A method of using microcontroller modular reaction device to prepare Vicprammonium bromide intermediate

A microchannel module, the technology of vecuronium bromide is applied in the field of chemical synthesis, can solve the problems of long reaction time, low yield, low selectivity, etc., and achieves the improvement of the conversion rate of raw materials, the reduction of side reactions, and the improvement of the yield of the preparation process Effect

Active Publication Date: 2016-11-30
NANJING TECH UNIV
View PDF3 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The technical problem to be solved by the present invention is that for 2β, 16β-dipiperidinyl-3α-hydroxyl-17-ketone-5α-androstane synthesis process has a long reaction time, low yield, low selectivity, and cannot be continuously produced. And proposed a kind of adopting microchannel modular reaction device to prepare vecuronium bromide intermediate 2β, the method of 16β-dipiperidinyl-3α-hydroxyl-17-ketone-5α-androstane

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • A method of using microcontroller modular reaction device to prepare Vicprammonium bromide intermediate
  • A method of using microcontroller modular reaction device to prepare Vicprammonium bromide intermediate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of method adopting microchannel modular reaction device to prepare vecuronium bromide intermediate, the method comprises the steps:

[0032] (1) Pump the piperidine solution of water and 2α, 3α-epoxy-16α-bromo-17-one-5α-androstane into the microchannel modular reaction device respectively, and control the 2α, 3α-epoxy-16α- The molar ratio of bromo-17-one-5α-androstane to piperidine is 1:15, and the molar ratio of 2α,3α-epoxy-16α-bromo-17-one-5α-androstane to water is 1: 20; Reaction residence time at 120°C is 35min;

[0033] (2) After the reaction finishes, the reaction solution is distilled under reduced pressure at 40° C. to remove water and piperidine;

[0034] (3) Dissolve the residual liquid after step (2) with 1mol / L dilute hydrochloric acid solution and adjust pH=3; The volume consumption is the same as the volume of water in the step (1), and the impurities are washed 3 times;

[0035] (4) The aqueous phase that step (3) obtains adjusts pH=9 with 20wt%...

Embodiment 2

[0038] A kind of method adopting microchannel modular reaction device to prepare vecuronium bromide intermediate, the method comprises the steps:

[0039](1) Pump the piperidine solution of water and 2α, 3α-epoxy-16α-bromo-17-one-5α-androstane into the microchannel modular reaction device respectively, and control the 2α, 3α-epoxy-16α- The molar ratio of bromo-17-one-5α-androstane to piperidine is 1:18, and the molar ratio of 2α,3α-epoxy-16α-bromo-17-one-5α-androstane to water is 1: 25; Reaction residence time at 135°C is 40min;

[0040] (2) After the reaction finishes, the reaction solution is distilled under reduced pressure at 40° C. to remove water and piperidine;

[0041] (3) Dissolve the residual liquid after step (2) with 1mol / L dilute hydrochloric acid solution and adjust pH=2; The volume consumption is the same as the volume of water in the step (1), and the impurities are washed 3 times;

[0042] (4) The aqueous phase that step (3) obtains is adjusted pH=10 with 2...

Embodiment 3

[0045] A kind of method adopting microchannel modular reaction device to prepare vecuronium bromide intermediate, the method comprises the steps:

[0046] (1) Pump the piperidine solution of water and 2α, 3α-epoxy-16α-bromo-17-one-5α-androstane into the microchannel modular reaction device respectively, and control the 2α, 3α-epoxy-16α- The molar ratio of bromo-17-one-5α-androstane to piperidine is 1:20, and the molar ratio of 2α,3α-epoxy-16α-bromo-17-one-5α-androstane to water is 1: 30; Reaction residence time at 140°C is 45 minutes;

[0047] (2) After the reaction finishes, the reaction solution is distilled under reduced pressure at 30°C to remove water and piperidine;

[0048] (3) Dissolve the residual liquid after step (2) with 1mol / L dilute hydrochloric acid solution and adjust pH=2; The volume consumption is the same as the volume of water in the step (1), and the impurities are washed 3 times;

[0049] (4) The aqueous phase that step (3) obtains is adjusted pH=10 wi...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a method for preparing a vecuronium bromide intermediate by employing a microchannel modularization reaction device. The method comprises the following steps: respectively pumping water and a piperidine solution of 2alpha,3alpha-epoxy-16alpha-bromine-17-ketone-5-alpha-androstane into the microchannel modularization reaction device; controlling the reaction temperature to be 100-150 DEG C and the reaction residence time to be 30-45 minutes in a micro-reactor of the microchannel modularization reaction device; after reacting, distilling reaction liquid at reduced pressure, and removing water and piperidine; dissolving the residual liquid with a dilute hydrochloric acid solution, and adjusting the pH value to be 2-3; adding dichloromethane to wash impurities, skimming, and taking an upper water phase; adjusting the pH value of the water phase to be 9-10 with a NaOH water solution, and extracting with dichloromethane; and drying the extracted organic phase with anhydrous sodium sulfate, and carrying out vacuum concentration, so as to obtain the vecuronium bromide intermediate 2beta,16beta-dipiperidino-3alpha-hydroxy-17-ketone-5alpha-androstane.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and relates to a method for preparing vecuronium bromide intermediate 2β, 16β-dipiperidinyl-3α-hydroxyl-17-ketone-5α-androstane by using a microchannel modular reaction device. Background technique [0002] Vecuronium bromide, the chemical name is 1-[3α,17β-diacetoxy-2β-(1-piperidinyl)-5α-androstane-16β-yl]-1-methyl bromide Piperidine, a monoquaternary ammonium steroid intermediate-effect non-depolarizing muscle relaxant, is mainly used as an adjuvant drug for general anesthesia, used for tracheal intubation during general anesthesia and muscle relaxation during surgery. This product has the characteristics of quick onset, short duration, no accumulation, no tachycardia and blood pressure changes, and no release of histamine. Vecuronium bromide is a category B variety of national medical insurance, and it is a key recommended variety for production and scientific research during the "...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
Patent Type & Authority Patents(China)
IPC IPC(8): C07J43/00
CPCC07J43/003
Inventor 郭凯方正王梦雪何伟欧阳平凯
Owner NANJING TECH UNIV
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap