96556-05-7Relevant articles and documents
Well-defined iron complexes as efficient catalysts for green atom-transfer radical polymerization of styrene, methyl methacrylate, and butyl acrylate with low catalyst loadings and catalyst recycling
Nakanishi, So-Ichiro,Kawamura, Mitsunobu,Kai, Hidetomo,Jin, Ren-Hua,Sunada, Yusuke,Nagashima, Hideo
, p. 5802 - 5814 (2014)
Environmentally friendly iron(II) catalysts for atom-transfer radical polymerization (ATRP) were synthesized by careful selection of the nitrogen substituents of N,N,N-trialkylated-1,4,9-triazacyclononane (R3TACN) ligands. Two types of structures were confirmed by crystallography: [(R3TACN)FeX2] complexes with relatively small R groups have ionic and dinuclear structures including a [(R 3TACN)Fe(μ-X)3Fe(R3TACN)]+ moiety, whereas those with more bulky R groups are neutral and mononuclear. The twelve [(R3TACN)FeX2]n complexes that were synthesized were subjected to bulk ATRP of styrene, methyl methacrylate (MMA), and butyl acrylate (BA). Among the iron complexes examined, [{(cyclopentyl) 3TACN}FeBr2] (4b) was the best catalyst for the well-controlled ATRP of all three monomers. This species allowed easy catalyst separation and recycling, a lowering of the catalyst concentration needed for the reaction, and the absence of additional reducing reagents. The lowest catalyst loading was accomplished in the ATRP of MMA with 4b (59ppm of Fe based on the charged monomer). Catalyst recycling in ATRP with low catalyst loadings was also successful. The ATRP of styrene with 4b (117ppm Fe atom) was followed by precipitation from methanol to give polystyrene that contained residual iron below the calculated detection limit (0.28ppm). Mechanisms that involve equilibria between the multinuclear and mononuclear species were also examined. It's easy being green: Structurally well-defined [(R3TACN)FeX 2] complexes realized green atom-transfer radical polymerization by judicious choice of the R group on the N,N,N-trialkylated-1,4,9- triazacyclononane (R3TACN) ligands (see scheme). [{(Cyclopentyl) 3TACN}FeBr2] was the best catalyst for controlled polymerization of all three monomers.
A method for preparing nitrogen heterocyclic
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Paragraph 0027; 0030, (2017/02/24)
The invention discloses a preparation method of azacyclo. The preparation method comprises the following steps of: (1) reacting diethylenetriamine or triethylene tetramine with methylsulfonyl chloride to generate methanesulfonamide; (2) during two-phase reaction, cyclizing compound catalytic cyclization on methanesulfonamide and a compound having the structure shown in a chemical formula (a) under the composite catalysis of benzyl triethylanmine compound and 15-crown-5 at 90 DEG C under a backflow condition; and (3) removing methylsulfonyl from methanesulfonamide azacyclo and performing methylation treatment, wherein X represents bromine, iodine or sulphonate. The preparation method has the advantages that raw materials are low in cost, atom economy is high, and operation is easy and safe. The preparation method is suitable for industrial production.
Method of producing polymer using iron complex as catalyst
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Page/Page column 17, (2010/04/23)
The object of the present invention is to provide a method of producing a polymer wherein radical-polymerizable monomers can be polymerized in a quantitative manner in a relatively short time, and a polymer or a block copolymer having at its termini a functional group that can be chemically converted while the polymer or the block copolymer has a high molecular weight can be produced. Furthermore, the object of the present invention is to provide a method of producing a polymer wherein the polymer is re-precipitated in a general solvent by an easy method, and the used iron complexes are recovered in the solvent, thereby recycling the iron complexes.