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

Compound, palladium compound and nickel compound as well as preparation methods thereof

A technology of palladium compounds and compounds, applied in nickel organic compounds, chemical instruments and methods, compounds of group 5/15 elements of the periodic table, etc., can solve problems such as low activity, low copolymer molecular weight, low insertion ratio, etc., and achieve Effects of high activity, high copolymer molecular weight, and high insertion ratio

Active Publication Date: 2018-05-11
UNIV OF SCI & TECH OF CHINA
View PDF2 Cites 5 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there have been extensive studies on such catalysts, many catalysts exhibit low activity, low copolymer molecular weight, low insertion ratio

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
  • Compound, palladium compound and nickel compound as well as preparation methods thereof
  • Compound, palladium compound and nickel compound as well as preparation methods thereof
  • Compound, palladium compound and nickel compound as well as preparation methods thereof

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0060] The present invention provides a kind of preparation method of the compound of formula (I) structure, comprising:

[0061] The compound of formula (II) is reacted with the compound of formula (III) to obtain the compound of formula (IV);

[0062] The compound of formula (IV) is reacted with the compound of formula (V) to obtain the compound of formula (I);

[0063]

[0064] where R 1 One or more selected from H, C1-C6 alkoxy, substituted C1-C6 alkyl, C1-C6 alkyl, dimethylamino, nitro, and halogen; the substitution of the substituted alkyl The base is fluorine;

[0065] R 2 , R 3 independently selected from substituted phenyl or substituted biphenyl; the substituent of the substituted phenyl is selected from one or more of C1-C6 alkoxy and C1-C10 alkyl; the substituted biphenyl The substituent of the group is selected from one or more of C1-C6 alkoxy and C1-C10 alkyl;

[0066] R 4 It is selected from C1-C6 alkyl group and C6-C12 aryl group.

[0067] Preferably...

Embodiment 1

[0134] Example 1 Preparation of N-((2-methoxyphenyl)-12-phosphoranyl)-N,P,P-triphenylphosphine amide

[0135]

[0136] Dissolve aniline (0.9 g, 10.0 mmol) in 100 ml of EtO at -78°C 2 Slowly add an equivalent to the solution n BuLi (2.5M in hexane, 4.4mL, 1.1eq) was stirred for 15min, reacted at room temperature for 1-2h, and an equivalent of compound Ph was added to it at -78°C 2 POCl (2.4 g, 10.0 mmol) was reacted at room temperature for 12 h, and the target product A was obtained by column chromatography (where A does not need to be characterized, and can be directly used as a raw material in the next step). To a solution of dissolved A (2.925 g, 10 mmol) in 100 ml of THF at 0°C was addedn BuLi (2.5M in hexane, 4.4mL, 1.1eq) was reacted at room temperature overnight, compound B (3.08g, 1eq) was added at -78°C, the reaction was carried out for 24h, and the target product formula L-1 was obtained by column chromatography. Use a rotary evaporator to spin dry, add DCM to di...

Embodiment 2

[0138] Example 2 N-((2',6'-dimethoxy-[1,1'-biphenyl]-2-yl)(phenyl)phosphono)-N,P,P-triphenylene Preparation of phosphonamides

[0139]

[0140] The steps were the same as above, aniline was added, and ArPhPCl (3.6 g, 10.0 mmol) was added in the fourth step to obtain a white solid (3.5 g, 65%).

[0141] 1 H NMR (400MHz, CDCl 3 ):δ8.00(dd,J=11.8,7.1Hz,4H),7.34(m,8H),7.22(t,J=7.7Hz,2H),7.03(d,J=7.2Hz,2H),6.83 (t, J=7.4Hz, 2H), 6.78 (dd, J=10.8, 5.3Hz, 3H), 6.67 (dd, J=8.0, 5.2Hz, 2H), 3.68 (s, 6H). 13 C NMR (101MHz, CDCl3): δ160.7(d, J PC =18.0Hz)141.5(d,J PC =4.0Hz),134.0(d,J PC =3.0Hz),133.7(d,J PC =3.0Hz),133.3(d,J PC =3.0Hz)133.2(d,J PC =3.0Hz),131.7(d,J PC = 3.0Hz), 130.9(s), 129.9(d, J PC =4.0Hz),128.1(d,J PC =3.0Hz), 128.0(s), 125.5(s), 124.6(d, J PC =4.0Hz)124.4(d,J PC = 4.0Hz), 120.6(s), 110.1(s), 55.6(s). 31 P NMR (CDCl 3 ,162MHz):δ45.7(d,J=75.3Hz),28.3(d,J=75.3Hz).ESI-MS(m / z):[M+H] + Calcd for C 32 H 30 NO 3 P 2 , 538.1701; Found: 538.1700.

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 provides a compound with a structure shown in a formula (I), wherein R1 is selected from one or more of H, C1-C6 alkoxy, substituted C1-C6 alkyl, C1-C6 alkyl, dimethylamino, nitryl and halogen, wherein a substituent group of substituted alkyl is fluorine; R2 and R3 are independently selected from substituted phenyl and substituted biphenylyl; R4 is selected from C1-C6 alkyl and C6-C12 aryl. The electron-withdrawing effect or shared electron effect of a specific R1 group in the structure of the formula (I) has an effect on polymerization activity, besides, in combination with different substituted groups on the phosphine oxide framework, large steric hindrance and other effects of aromatic groups substituted by the substituent group jointly show high polymerization activity, the compound has ethylene homopolymerization molecular weight up to 188,900, wherein the ethylene and MA copolymerization molecular weight is up to 20,700. Therefore, the prepared compound is a polyolefin catalyst with high activity, high molecular weight of copolymer and high insertion ratio.

Description

technical field [0001] The invention relates to the technical field of organic synthesis, in particular to a compound, a palladium compound, a nickel compound and a preparation method thereof. Background technique [0002] Since the discovery of coordination polymerization catalysts by Ziegler in 1953, olefin polymerization technology has maintained a rapid development, from catalysts, polymerization methods to polymerization processes, about every ten years, there will be a major breakthrough in technology, or Reduce the production cost of polyolefins, or bring newer, wider and higher properties to polyolefins. [0003] In olefin polymerization, catalysts determine olefin polymerization behavior, polymer structure and properties, and polymer particle morphology. The development of olefin polymerization catalysts makes polyolefin products rich in variety and excellent in performance, which promotes the development of the entire polyolefin. [0004] Olefin polymerization ca...

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): C07F9/36C07F9/46C07F15/00C07F15/04C08F4/80C08F210/02C08F110/02C08F2/34C08F216/14C08F220/14C08F220/06
Inventor 陈昶乐陈敏
Owner UNIV OF SCI & TECH OF CHINA
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