Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Preparation method of cyclopropyl acetylene

A technology of cyclopropyl acetylene and cyclopropane ketone, which is applied in the field of preparation of cyclopropyl acetylene, can solve problems such as waste of resources and environmental pollution, and achieve the effects of less environmental pollution, reduced pollution and simple process

Active Publication Date: 2017-01-04
裴卿
View PDF10 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Waste polyester bottles enter the environment and cannot be degraded spontaneously, which will cause serious environmental pollution and waste of resources. Therefore, waste polyester bottles and other polyester packaging must be recycled

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
  • Preparation method of cyclopropyl acetylene

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0016] Preparation of reaction medium:

[0017] Take a certain amount of crushed waste polyester bottle material, add methanol solution to at least submerge the waste polyester bottle material, heat and reflux until the waste polyester bottle material is completely dissolved, filter out the insoluble matter while it is hot, and obtain a mixture after alcoholysis [(methyl terephthalate (DMT) and ethylene glycol (EG))] for the following reaction.

Embodiment 1

[0019] In the reactor, add 84 grams (1 mole) of cyclopropyl ketone, 208.5 grams (1 mole) of phosphorus pentachloride, utilize the mixture [methyl terephthalate (methyl terephthalate ( DMT) and ethylene glycol (EG)] 404.5 grams, stirred and reacted for 5 hours at a temperature of 0°C, added 112 grams (2 moles) of potassium hydroxide, continued to stir and react at the same temperature, and gas chromatographic tracking was detected until the end of the reaction. After filtering off the solid matter, 49 g of the product was purified by rectification, with a yield of 74%, a boiling point of 52-53°C, and a cyclopropylacetylene content of ≥98% as determined by HPLC.

Embodiment 2

[0021] In the reactor, add 84 grams (1 mole) of cyclopropyl ketone, 417 grams (2 moles) of phosphorus pentachloride, utilize the mixture [methyl terephthalate (methyl terephthalate ( DMT) and ethylene glycol (EG)] 2000 grams, stirred and reacted at -5 ℃ for 5 hours, added 224 grams (4 moles) of potassium hydroxide, continued to stir and react at the same temperature, and gas chromatography tracked and detected until the end of the reaction. After filtering off the solid matter, 48 g of the product was purified by rectification, with a yield of 73%, a boiling point of 52-53°C, and a cyclopropylacetylene content of ≥98% as determined by HPLC.

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

PropertyMeasurementUnit
Boiling pointaaaaaaaaaa
Login to View More

Abstract

The invention discloses a preparation method of cyclopropyl acetylene. The preparation method comprises the following steps: with cyclopropyl methyl ketone and phosphorus pentachloride as raw materials as well as dimethyl terephthalate and ethylene glycol which are obtained through alcoholysis of a waste polyester material in a methanol solution as reaction mediums, carrying out reaction under stirring at (-10)-0 DEG C for 1-10 hours, adding potassium hydroxide, carrying out the reaction under stirring at the same temperature, carrying out gas chromatography tracking and detection until the reaction is finished, filtering out solids, and carrying out rectification and purification, so as to obtain the product, namely cyclopropyl acetylene. According to the preparation method, dimethyl terephthalate (DMT) and ethylene glycol (EG) which are obtained through alcoholysis of the waste polyester material in the methanol solution are taken as the reaction mediums so as to prepare cyclopropyl acetylene by virtue of a one-pot method reaction technique, so that the process is simple and convenient, the operation is easy, the emission of three wastes is reduced, the environmental pollution is low, and the preparation method is an environment-friendly and clean comprehensive utilization production process and is suitable for industrial production in a certain scale. The preparation method has not been reported, and a new thought is provided for the preparation of cyclopropyl acetylene.

Description

technical field [0001] The invention relates to a preparation method for synthesizing a key intermediate of cyclopropylacetylene for treating AIDS. Background technique [0002] Cyclopropylacetylene is a key intermediate of some AIDS drugs and an important intermediate of the non-nucleoside reverse transcriptase inhibitor efavirenz. Cyclopropylacetylene, as an important synthon of the cyclopropyl skeleton of such drug molecules, has quickly become the focus of research. In recent years. The research on AIDS drugs has made gratifying achievements, such as Merck, Kumray, DuPont, Wiley, etc. have developed effective drugs for the treatment of AIDS. Cyclopropylacetylene is an important intermediate, and the development and research of cyclopropylacetylene's industrial production technology has broad application prospects. [0003] At present, the existing process mainly uses cyclopropyl methyl ketone, cyclopropyl methyl aldehyde, 5-chloro-1-pentyne and other alkyne-containing...

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): C07C13/04C07C1/30
CPCC07C1/30C07C17/18C07C13/04C07C22/00
Inventor 裴卿
Owner 裴卿
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com