Unlock instant, AI-driven research and patent intelligence for your innovation.

Synthetic process for trimethylsilyl acetylene

A technology of trimethylsilyl acetylene and synthesis process, applied in the direction of silicon organic compounds, etc., can solve the problems of complex synthesis method, difficult to obtain raw materials, high price, and achieve the effect of simple and convenient purification

Active Publication Date: 2010-12-22
HAIMEN RUIYI MEDICAL TECH +1
View PDF2 Cites 4 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the raw materials used in the current synthetic method of trimethylsilylacetylene are generally difficult to obtain, and the price is high, and the synthetic method is complicated

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
  • Synthetic process for trimethylsilyl acetylene
  • Synthetic process for trimethylsilyl acetylene
  • Synthetic process for trimethylsilyl acetylene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Suspend 1kg of sodium acetylide in 5L of ether, under the protection of nitrogen, slowly add trimethylchlorosilane dropwise at 0°C, the dropwise addition is completed in about 4 hours, slowly heat up to reflux for 8 hours, cool to room temperature, and drop into the reaction solution Add 500ml of ice water to quench the reaction. The ether phase was washed with saturated brine (500ml×3), dried and filtered. 10 × 150cm packing column atmospheric pressure rectification collects the fraction with a boiling point of about 45 degrees, and the yield is about 75%.

Embodiment 2

[0020] Take 1kg of acetylene lithium ethylenediamine and dissolve it in 5L of DMSO. Under the protection of nitrogen, slowly add trimethylchlorosilane dropwise at 0°C. The dropwise addition is completed in about 1 hour. Slowly warm up to room temperature and react for 2 hours. Cool to room temperature and proceed to the reaction. 500ml of ice water was added dropwise to quench the reaction. 500mL×3 diethyl ether was extracted, dried and filtered, and the distillate with a boiling point of about 45 degrees was collected by a 10×150cm packed column at atmospheric pressure, with a yield of about 60%.

Embodiment 3

[0022] A synthesis process of trimethylsilylacetylene, the method is to slowly drop trimethylchlorosilane into the ether suspension or solution of sodium acetylide, and reflux reaction at 25°C for 10 hours, wherein sodium acetylide and trimethyl chloride The molar ratio of silane is between 1:1. After the reaction is finished, it is washed with water, and the fraction near the boiling point of the product is collected by atmospheric distillation to obtain the product. The product obtained is washed with a large amount of water to remove inorganic salts for post-treatment. The reaction formula is as follows:

[0023]

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 relates to a synthetic process for trimethylsilyl acetylene. The process comprises the following steps of: slowly dripping trimethyl halogenosilane into organic solvent suspension or solution of acetylene metal compound, and performing reflux reaction for 6 to 12 hours, wherein the molar ratio of the acetylene metal compound to the trimethyl halogenosilane is between 0.9:1 and 1.2:1; and slowly adding water into the reaction product after the reaction is finished, performing quenching reaction, and collecting distillates nearby a product boiling point by rectification to obtain a product. Compared with the prior art, the process has the advantages of easily obtained raw material, simple and convenient operation and the like.

Description

technical field [0001] The invention relates to a pharmaceutical intermediate, in particular to a synthesis process of trimethylsilylacetylene. Background technique [0002] As the most commonly used alkyne reagent, trimethylsilylacetylene has always had a very broad market demand. Trimethylsilylacetylene is mainly used for Sonagoshi coupling reaction with aryl halides to generate aryne, which is an important method for preparing aryne. However, the raw materials used in the current synthetic method of trimethylsilylacetylene are generally difficult to obtain, and the price is high, and the synthetic method is complicated. Contents of the invention [0003] The object of the present invention is to provide a synthesis process of trimethylsilylacetylene with easy-to-obtain raw materials and easy operation in order to overcome the above-mentioned defects in the prior art. [0004] The object of the present invention can be achieved through the following technical solutions...

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
IPC IPC(8): C07F7/08
Inventor 薛嵩
Owner HAIMEN RUIYI MEDICAL TECH
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More

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

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com