Method for synthesizing polypren phosphate

A technology of polypentenyl phosphate and synthesis method, applied in the direction of phosphorus organic compounds, etc., to achieve the effect of simple source

Inactive Publication Date: 2005-12-21
INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
View PDF1 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no research report on the synthesis method and application of plant polyprenol phosphate in China

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
  • Method for synthesizing polypren phosphate
  • Method for synthesizing polypren phosphate
  • Method for synthesizing polypren phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0060] A kind of polypentenyl phosphate synthetic method, comprises the following steps:

[0061] In the first step, an oily substance with a plant polyprenol content higher than 85%, for example, a plant polyprenol content of 90%, is added to a non-polar organic solvent to form a mixed solution, and phosphorus is catalyzed by a nitrogen-containing organic base. Add the acylating agent dropwise to the above mixed solution, and stir at a speed of 50-800rpm while adding dropwise. The stirring speed can be selected as 100rpm, 350rpm, or 740rpm. °C, 25 °C, 36 °C, 48 °C, 55 °C, 62 °C, 74 °C, 79 °C, and make the reactant in a vacuum of 50-200 mmHg, for example, the vacuum can be selected as 100 mmHg, 160 mmHg After the dropwise addition, continue to react for 1 to 4 hours. For example, the reaction time can be selected as 1.2 hours, 2.5 hours, and 3.4 hours to obtain a mixed solution containing the reaction product.

[0062] Wherein, the structure of plant polyprenol is (H 3 c) 2...

Embodiment 2

[0067] Synthesis of Polypentenyl Phosphate Monoester Using Pyrophosphoric Acid as Phosphorylating Agent

[0068] Take 5 g of refined polyprenol samples, dissolve them in 70 ml of carbon tetrachloride solution, and transfer them to a 250 ml three-neck flask. Take 3.5g of pyrophosphoric acid solution, add it to 70ml of carbon tetrachloride solution, and then slowly drop it into the reactor for reaction, the dropping rate is 1-5ml / min., the reaction temperature is 50°C-60°C, and the stirring speed is 100-800r / min. Min, the vacuum degree is 50-200mmHg, after 2 hours of reaction, add 3 grams of triethylamine, continue the reaction for 1-2 hours, then add 80ml of acetone, 20ml of water and 0.5ml of triethylamine to carry out catalytic and hydrolysis reactions. The reaction temperature is 65°C-75°C, the stirring speed is 100-800r / min, the vacuum degree is 50-200mmHg, and the reaction time is 1-2 hours. Stop the reaction, add 100ml of water and 0.5ml of triethylamine after cooling, e...

Embodiment 3

[0070] Synthesis of Polypentenyl Dichlorophosphate Using Phosphorus Oxychloride as Phosphorylation Agent

[0071] Take 5 g of refined polyprenol samples and dissolve them in 100 ml of n-hexane solution. Take POCl 3 Dissolve 2.8ml of solvent in 100ml of n-hexane solution, transfer it to a 500ml three-neck flask, stir under ice bath at a stirring speed of 100-800r / min, dissolve 4.2ml of triethylamine in 30ml of n-hexane solution, slowly add triethylamine dropwise Put the amine n-hexane solution into the reactor at a rate of 1-5ml / min. During the dropping process, when a large amount of white mist is generated, stir in vacuum at a stirring speed of 100-800r / min, with a vacuum degree greater than 600mmHg, and react for 30min.

[0072] Then slowly drop 100ml of polypentenol n-hexane solution into the reactor, the dropping speed is 1-5ml / min., the stirring speed is 50-800r / min, react in ice bath for 1 hour, and the reaction product is polypentenyl chlorophosphoric acid Esters mixt...

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

This invention has disclosed a manufacturing method for polypentenyl phosphate. Put oil of plant polyprenol into nonpolar organic solvent, formed a mix solution, under the nitric organic alkali catalysis, put phosphorylation agent into above-mentioned mix solution, mix, get mixture contained reaction products, put hydrolysis liquid into the mixture, mixing for 1-2 hours, then evaporation, retrieve the organic solvent, the hangover is mainly emulsion of polypentenyl phosphate. Extract above-mentioned emulsion with the solvent to separate, volume ratio of emulsion and solvent is 1:(5-100), the solvent is mixture of nonpolar organic solvent and water, ratio of nonpolar organic solvent and water is (1-10):1, mixing for 1-10 hours, then wait 1-10 hours quietly for delamination, wash the supernatant with saturated inorganic sodium salt solution again and again to neutrality, recovery nonpolar organic solvent in the supernatant, gained yellow oil of polypentenyl phosphate.

Description

technical field [0001] The invention relates to a synthesis of organic esters, in particular to a synthesis method of polypentenyl phosphate. Background technique [0002] Plant polyprenols widely exist in higher plants and are a class of lipid compounds composed of a series of prenyl units and terminal prenol units. According to the number of polypentenyl units and the connection methods of cis (cis) and trans (trans) prenyl groups, plant polyprenyl alcohols are divided into three types, one is the all-trans structure ω-(trans)n- OH (n=7-18), including Solanesol isolated from tobacco leaves and pine polyprenol isolated from Scots pine. The second type is polyprenyl alcohol with two isopentenyl trans configuration (trans) units in the molecule and the rest are cis configuration (cis) units, that is, ω-(trans)2-(cis) n-α (wherein n is 11-19, and α is prenol). The third type is that there are three isopentenyl trans (trans) units in the molecule, an...

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 Applications(China)
IPC IPC(8): C07F9/09
Inventor 王成章沈兆邦刘妤婵
Owner INST OF CHEM IND OF FOREST PROD CHINESE ACAD OF FORESTRY
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