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

Method for synthesizing tetrakis(triphenylphosphine)palladium by liquid-phase crystallization and application of tetrakis(triphenylphosphine)palladium in emamectin benzoate production

A technology of tetrakistriphenylphosphine palladium and triphenylphosphine, which is applied in the production process field of tetrakistriphenylphosphine palladium, can solve problems such as easy oxidation, low production efficiency, and product purity to be improved, and achieve high product purity and easy saved effect

Pending Publication Date: 2021-04-02
内蒙古新威远生物化工有限公司
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Among them, in the C-5 deprotection reaction, it is necessary to use tetrakistriphenylphosphine palladium as a catalyst, and the traditional production process of tetrakistriphenylphosphine palladium has problems such as low production efficiency and easy oxidation during the production process, and the product purity still needs to be improved

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 tetrakis(triphenylphosphine)palladium by liquid-phase crystallization and application of tetrakis(triphenylphosphine)palladium in emamectin benzoate production
  • Method for synthesizing tetrakis(triphenylphosphine)palladium by liquid-phase crystallization and application of tetrakis(triphenylphosphine)palladium in emamectin benzoate production

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] This embodiment provides a method for synthesizing tetrakistriphenylphosphine palladium by liquid phase crystallization. The specific synthesis method is as follows:

[0026] 16g palladium chloride and 133g triphenylphosphine were dissolved in 666.5mlDMF, in N 2 Under the protection of the oil bath, the oil bath was heated to 150°C to reflux, the solution was brown and turbid, and the heating was stopped after the temperature reached 150°C. 2 Under the protection, start to add hydrazine hydrate dropwise, control the drop rate, and ensure that the temperature reaches 130°C after the dropwise addition is completed. At this time, the solution is in a light brown and transparent state. At this time, the temperature is naturally cooled to 30-40°C, and green crystals are precipitated. 2 Suction filtration was started under protection, and after solid-liquid separation was achieved, the crystals were rinsed with petroleum ether, and after drying in the air, tetrakistriphenylph...

Embodiment 2

[0028] Synthetic tetrakistriphenylphosphine palladium according to embodiment one, present embodiment provides a kind of synthetic tetraphenylphosphine palladium with embodiment one as catalyst, carries out the C of the synthetic technique of emamectin benzoate -5 deprotection reaction.

[0029] Add 256 g of methanol to the dichloromethane solution (about 0.83 moles of active ingredient) of abamectin with a C-5 protecting group, and add 9.6 g of sodium borohydride dropwise at -5°C to 5°C under temperature control. After the dropwise addition, add 160g of methanol and 0.1g of the prepared tetrakistriphenylphosphine palladium, control the temperature at -5°C to 5°C, add 11.2g of sodium borohydride dropwise, and check the reaction progress by high-pressure liquid chromatography after the dropwise addition. as attached figure 2 The shown results show that: 5.582min is the main peak of emamectin.

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 method for synthesizing tetrakis(triphenylphosphine)palladium through liquid-phase crystallization and application of tetrakis(triphenylphosphine)palladium in emamectin benzoate production. The method for synthesizing tetrakis(triphenylphosphine)palladium through liquid-phase crystallization comprises the steps of 1, placing DMF in a reactor, adding palladium chloride and triphenylphosphine into the reactor, introducing N2 for protection, and conducting oil bath heating to the temperature of 140-160 DEG C for backflow; 2, dropwise adding hydrazine hydrate into the solution obtained after the reaction in the step 2, controlling the dropwise adding speed, ensuring that the temperature is reduced to 110-140 DEG C after dropwise adding is completed, then naturally cooling to the temperature of 20-40 DEG C, and separating out green crystals; 3, carrying out suction filtration under the protection of N2 to obtain a wet crystal with DMF; 4, leaching the wet crystalobtained in the step 3 by using petroleum ether under the protection of N2, and airing to obtain tetrakis(triphenylphosphine)palladium; and 5, sub-packaging the prepared tetrakis(triphenylphosphine)palladium for later use. The process disclosed by the invention has the advantages of environmental protection, high efficiency, high product purity, easiness in storage and the like.

Description

technical field [0001] The invention relates to a production process of tetrakistriphenylphosphine palladium, in particular to a method for synthesizing tetrakistriphenylphosphine palladium by liquid phase crystallization and its application in the production of emamectin benzoate. Background technique [0002] The development of abamectin has a history of decades. In 1991, Merck obtained the temporary registration of abamectin in my country, and the research on abamectin in my country began in 1984. The research on abamectin And industrial production is listed as a national key scientific and technological project. After continuous research, the shake flask fermentation unit of abamectin has been improved in quality, driven by scientific and technological progress and driven by market demand, making the abamectin industry continue to grow in my country and become the fastest growing variety in the field of pesticides in China. Since 2007, abamectin, a "noble product", has c...

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): C07F9/50C07H17/08C07H1/06B01J31/24
CPCC07F9/5045C07H17/08C07H1/06B01J31/2409B01J2531/824Y02P20/55
Inventor 王韬张强齐殿巍杨军强徐龙广韩悦
Owner 内蒙古新威远生物化工有限公司