583-55-1Relevant articles and documents
Preparation method 2 - bromoiodobenzene
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Paragraph 0024-0037, (2021/08/25)
The invention discloses a preparation method of 2 -bromoiodobenzene, which comprises the following steps: under the protection of inert gas, adding triphenylphosphine to an organic solvent, adding organic amine to 50 - 75 °C DEG C under stirring conditions, and stirring 1 - 2 hours. Then iodine is added to 60 - 80 °C thermal insulation stirring 2 - 4.5 hours. Finally 2 - bromophenol was added and stirred 5 - 10 hours under reflux. The resulting reaction solution was naturally cooled to ≤ 40 °C, sodium methoxide was added, stirred and filtered, and the filtrate was post-treated to give 2 - bromoiodobenzene. 2 - Bromoiodobenzene is prepared by the method disclosed by the invention, and has the characteristics of simple process and high product yield.
Metathesis-active ligands enable a catalytic functional group metathesis between aroyl chlorides and aryl iodides
Lee, Yong Ho,Morandi, Bill
, p. 1016 - 1022 (2018/09/06)
Current methods for functional group interconversion have, for the most part, relied on relatively strong driving forces which often require highly reactive reagents to generate irreversibly a desired product in high yield and selectivity. These approaches generally prevent the use of the same catalytic strategy to perform the reverse reaction. Here we describe a catalytic functional group metathesis approach to interconvert, under CO-free conditions, two synthetically important classes of electrophiles that are often employed in the preparation of pharmaceuticals and agrochemicals—aroyl chlorides (ArCOCl) and aryl iodides (ArI). Our reaction design relies on the implementation of a key reversible ligand C–P bond cleavage event, which enables a non-innocent, metathesis-active phosphine ligand to mediate a rapid aryl group transfer between the two different electrophiles. Beyond enabling a practical and safer approach to the interconversion of ArCOCl and ArI, this type of ligand non-innocence provides a blueprint for the development of a broad range of functional group metathesis reactions employing synthetically relevant aryl electrophiles.
Copper-Free Double Silylation of 1,2-Dibromobenzenes Using a Mg/LiCl/DMI System
Kitamura, Tsugio,Yamada, Rin,Gondo, Keisuke,Eguchi, Nobuo,Oyamada, Juzo
, p. 2495 - 2500 (2017/05/22)
The reaction of 1,2-dibromobenzenes with chlorotrimethylsilane efficiently proceeded in the presence of Mg and LiCl in DMI under mild conditions, giving 1,2-bis(trimethylsilyl)benzenes in good to high yields. The reaction of 1,2-dibromobenzenes with chlorodimethylsilane under the same conditions afforded the corresponding 1,2-bis(dimethylsilyl)benzenes in high yields. Functional group transformations of 1,2-bis(trimethylsilyl)benzene were conducted to demonstrate the synthetic utility.