scholarly journals Cross-Coupling Biarylation of Nitroaryl Chlorides Through High Speed Ball Milling

2015 ◽  
Vol 3 (6) ◽  
pp. 12-35
Author(s):  
Solita Lam ◽  
Yvonne Puplampu Dove ◽  
Adrienne Morris ◽  
Ayunna Epps ◽  
Ghislain R Mandouma
Keyword(s):  
Ball Milling ◽  
High Speed ◽  
Coupling Reaction ◽  
Cross Coupling ◽  
Reaction Cross ◽  
Extraction And Purification ◽  
Custom Made ◽  
Ball Milling Technique ◽  
Solvent Free Reaction ◽  
High Speed Ball Milling

Solvent-free reaction using a high-speed ball milling technique has been applied to the classical Ullmann coupling reaction. Cross-coupling biarylation of several nitroaryl chlorides was achieved in good yields when performed in custom-made copper vials through continuous shaking without additional copper or solvent. Cross-coupling products were obtained almost pure and NMR-ready. These reactions were cleaner than solution phase coupling which require longer reaction time in high boiling solvents, and added catalysts as well as lengthy extraction and purification steps. Gram quantities of cross biaryl compounds have been synthesized with larger copper vials, a proof that this method can be used to reduce industrial waste and for sustainability.

scholarly journals Synthesis of Substituted 2,2’-Dinitrobiphenyls by a Novel Solvent-Free High Yielding Ullmann Coupling Biarylation:

2014 ◽  
Vol 2 (12) ◽  
pp. 133-149
Author(s):  
Ghislain R Mandouma ◽  
Ayunna Epps ◽  
John Barbas
Keyword(s):  
High Speed ◽  
Copper Catalyst ◽  
Coupling Reaction ◽  
Solvent Free ◽  
Extraction And Purification ◽  
Custom Made ◽  
Solid Nmr ◽  
Ball Milling Technique ◽  
First Time ◽  
Ullmann Coupling

Solvent-free reaction using a high-speed ball milling technique has been applied to the classical Ullmann coupling reaction for the first time. Biarylation of 2-iodonitrobenzene was achieved in quantitative yield when performed in a custom-made copper vial through continuous shaking without additional copper or solvent. The product was solid, NMR ready and required no lengthy extraction for purification. This reaction was cleaner, and faster than solution phase coupling which requires longer reaction time in high boiling solvents, added copper catalyst, and lengthy extraction and purification steps. Gram quantities of the biaryl compound were synthesized in larger copper vials. This is a general method that can be used to effectively reduce industrial waste en route to sustainability.

Solvent-free Sonogashira coupling reaction via high speed ball milling

2009 ◽  
Vol 11 (11) ◽  
pp. 1821 ◽  
Author(s):  
Dennis A. Fulmer ◽  
William C. Shearouse ◽  
Shareika T. Medonza ◽  
James Mack
Keyword(s):  
Ball Milling ◽  
High Speed ◽  
Coupling Reaction ◽  
Solvent Free ◽  
Sonogashira Coupling ◽  
Sonogashira Coupling Reaction ◽  
High Speed Ball Milling

ChemInform Abstract: Solvent-Free Sonogashira Coupling Reaction via High Speed Ball Milling.

ChemInform ◽  
2010 ◽  
Vol 41 (12) ◽  
Author(s):  
Dennis A. Fulmer ◽  
William C. Shearouse ◽  
Shareika T. Medonza ◽  
James Mack
Keyword(s):  
Ball Milling ◽  
High Speed ◽  
Coupling Reaction ◽  
Solvent Free ◽  
Sonogashira Coupling ◽  
Sonogashira Coupling Reaction ◽  
High Speed Ball Milling

Semiconductor Pb2P2S6 and size-dependent band gap energy of its nanoparticles

RSC Advances ◽  
2014 ◽  
Vol 4 (65) ◽  
pp. 34288-34293 ◽  
Author(s):  
Xian Zhang ◽  
Jianqiao He ◽  
Wei Chen ◽  
Chao Wang ◽  
Chong Zheng ◽  
...  
Keyword(s):  
Optical Properties ◽  
Band Gap ◽  
Ball Milling ◽  
High Speed ◽  
Size Dependence ◽  
Band Gap Energy ◽  
Gap Energy ◽  
Size Dependent ◽  
Ball Milling Technique ◽  
High Speed Ball Milling

Microcrystalline Pb2P2S6 powder was synthesized via a traditional melting salt method. The nanostructured Pb2P2S6 powder was further synthesized by a high-speed ball milling technique. The optical properties of the Pb2P2S6 powder show a size-dependence, with the band gap ranging from 2.56 eV to 2.88).

scholarly journals Flow Process Development and Optimization of A Suzuki-Miyaura Cross Coupling Reaction using Response Surface Methodology

2020 ◽  
Vol 15 (3) ◽  
pp. 604-616
Author(s):  
Girish Basavaraju ◽  
Ravishankar Rajanna
Keyword(s):  
Response Surface Methodology ◽  
Response Surface ◽  
Flow Reactor ◽  
Phenylboronic Acid ◽  
Coupling Reaction ◽  
Cross Coupling ◽  
Flow Process ◽  
Cross Coupling Reaction ◽  
Custom Made ◽  
Good Agreement

A custom-made tubular flow reactor was utilized to develop a mathematical model and optimize the Suzuki-Miyaura cross coupling reaction. In this study, the experimentation was designed and executed through the statistical design of experiments (DoE) approach via response surface methodology. The effect of molar ratios of phenylboronic acid (1) and 4-bromophenol (2), temperature, the catalyst tetrakis(triphenylphosphine)palladium, and equivalence of aqueous tripotassium phosphate was studied in detail. The flow reactor profile was in good agreement with batch conditions and significant improvements to the overall reaction time and selectivity towards desired [1-1-biphenyl]-4-ol (3) was achieved. The Suzuki coupling reaction in batch condition would take on an average of 4 to 6 hours to complete, which was effectively accomplished in 60 to 70 minutes in this tubular reactor setup and could be operated continuously. The reaction model is in good agreement with the reaction conditions. Copyright © 2020 BCREC Group. All rights reserved 

Mechanochemical palladium-catalyzed C(sp2)–H homocoupling of N-arylcarbamates: synthesis of 2,2′-biaryldiamines

2018 ◽  
Vol 5 (13) ◽  
pp. 2103-2107 ◽  
Author(s):  
Yiyi Weng ◽  
Tianwen Lan ◽  
Chen Sun ◽  
Ting Yang ◽  
Weike Su ◽  
...  
Keyword(s):  
Ball Milling ◽  
High Speed ◽  
Palladium Catalyzed ◽  
Weakly Coordinating ◽  
High Speed Ball Milling

The palladium-catalyzed dehydrogenative C(sp2)–H homocoupling of N-arylcarbamates under high-speed ball-milling conditions has been achieved using weakly coordinating directing groups, providing access to a variety of 2,2′-biaryldicarbamates.

ChemInform Abstract: Mechanically Activated Synthesis of 1,3,5-Triaryl-2-pyrazolines by High Speed Ball Milling.

ChemInform ◽  
2009 ◽  
Vol 40 (28) ◽  
Author(s):  
Xingyi Zhu ◽  
Zhenhua Li ◽  
Can Jin ◽  
Li Xu ◽  
Qianqian Wu ◽  
...  
Keyword(s):  
Ball Milling ◽  
High Speed ◽  
High Speed Ball Milling

Novel Mechanochemical Synthesis of Carbon Nanomaterials by a High-Speed Ball-Milling

2011 ◽  
Vol 284-286 ◽  
pp. 755-758 ◽  
Author(s):  
Satoshi Ohara ◽  
Zhenquan Tan ◽  
Hiroya Abe
Keyword(s):  
Ball Milling ◽  
Gas Phase ◽  
Carbon Nanostructures ◽  
High Speed ◽  
Collision Energy ◽  
Carbon Nanomaterials ◽  
Milling Process ◽  
Phase Reaction ◽  
Steel Balls ◽  
High Speed Ball Milling

A novel mechanochemical approach to produce sophisticated carbon nanomaterials is reported. It is demonstrated that carbon nanostructures such as carbon nanotubes and carbon onions are synthesized by high-speed ball-milling of steel balls. It is considered that the gas-phase reaction takes place around the surface of steel balls under local high temperatures induced by the collision energy in ball-milling process, which results in phase separated unique carbon nanomaterials.

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