- Method for synthesizing alkyl peroxycarboxylate by using titanium silicalite molecular sieve composite catalyst
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The invention relates to a method for synthesizing alkyl peroxycarboxylate by using a titanium silicalite molecular sieve composite catalyst, and belongs to the technical field of peroxide production. The method overcomes the defects in the prior art, and adopts the titanium silicalite molecular sieve and aluminosilicate molecular sieve composite catalyst to synthesize the alkyl peroxycarboxylate. In the chemical reaction process that tert-butyl hydroperoxide or tert-amyl hydroperoxide reacts with carboxylic acid to generate tert-butyl peroxycarboxylate or tert-amyl peroxycarboxylate, reaction water is generated. The reaction water needs to be removed from the reaction mixture in time. Azeotropic distillation and molecular distillation dehydration are generally adopted. However, these process operations require a high temperature, and are not conducive to the stabilization and safety of alkyl peroxycarboxylate. The catalyst disclosed by the invention contains the aluminosilicate molecular sieve, so that water generated by reaction can be adsorbed in time, and the synthesis reaction can be smoothly completed.
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Paragraph 0057-0062
(2021/04/10)
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- Method for producing alkyl peroxycarboxylate based on titanium silicalite molecular sieve composite catalyst
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The invention relates to a method for synthesizing alkyl peroxycarboxylate based on a titanium silicalite molecular sieve composite catalyst, and belongs to the technical field of peroxide production. According to the method, the defects in the prior art are overcome, and alkyl peroxycarboxylate is synthesized by adopting a titanium silicalite molecular sieve and a metal oxide composite catalyst. In the chemical reaction process that tert-butyl hydroperoxide or tert-amyl hydroperoxide reacts with carboxylic acid to generate tert-butyl peroxycarboxylate or tert-amyl peroxycarboxylate, reaction water is generated. The reaction water is to be removed from the reaction mixture in time. Azeotropic distillation and molecular distillation dehydration are generally adopted. However, these process operations require higher temperatures, which are not conducive to the stabilization and safety of alkyl peroxycarboxylate. The catalyst disclosed by the invention contains metal oxide, so that water generated by reaction can be adsorbed in time, and the synthesis reaction can be smoothly completed.
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Paragraph 0058-0061
(2021/04/17)
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- Bu4NI-Catalyzed, Radical-Induced Regioselective N-Alkylations and Arylations of Tetrazoles Using Organic Peroxides/Peresters
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Bu4NI-catalyzed regioselective N2-methylation, N2-Alkylation, and N2-Arylation of tetrazoles have been achieved using tert-butyl hydroperoxide (TBHP) as the methyl source, alkyl diacyl peroxides as the primary alkyl source, alkyl peresters as the secondary and tertiary alkyl sources, and aryl diacyl peroxides as the arylating source. These reactions proceed without pre-functionalization of tetrazole and in the absence of any metal catalysts. Here, peroxides serve the dual role of oxidants as well as alkylating or arylating agents. Based on DFT calculations, it was found that spin density, transition-state barriers (kinetic control), and thermodynamic stability of the products (thermodynamic control) play essential roles in the observed regioselectivity during N-Alkylation. This radical-mediated process is amenable to a broad range of substrates and provides products in moderate to good yields.
- Ghosh, Subhendu,Mir, Bilal Ahmad,Patel, Bhisma K.,Rajamanickam, Suresh,Sah, Chitranjan,Sethi, Garima,Venkataramani, Sugumar,Yadav, Vinita
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p. 2118 - 2141
(2020/03/13)
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- Iron-Catalyzed Vinylic C?H Alkylation with Alkyl Peroxides
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A variety of alkyl peresters and alkyl diacyl peroxides, which are readily accessible from carboxylic acids, are utilized as general primary, secondary, and tertiary alkylating reagents for iron-catalyzed vinylic C?H alkylation of vinyl arenes, dienes, and 1,3-enynes. This transformation affords olefinic products in up to 98 % yield with high E/Z values. A broad range of functionalities, including carboxyl, boronic acid, methoxy, ester, amino, and halides, are tolerated. This protocol provides a facile approach to some olefins that are difficult to access, and hence, offers an alternative to existing systems. The synthetic utility of this method is demonstrated by late-stage functionalization of selected natural-product derivatives.
- Ge, Liang,Jian, Wujun,Zhou, Huan,Chen, Shaowei,Ye, Changqing,Yu, Fei,Qian, Bo,Li, Yajun,Bao, Hongli
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supporting information
p. 2522 - 2528
(2018/08/01)
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- Iron-Catalyzed Radical Decarboxylative Oxyalkylation of Terminal Alkynes with Alkyl Peroxides
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An iron-catalyzed oxyalkylation of alkynes with alkyl peroxides as the alkylating reagents has been investigated. Alkyl peroxides are readily available from aliphatic acids and serve simultaneously as the alkylating reagents and internal oxidants. Primary, secondary, and tertiary alkyl groups of aliphatic acids were readily incorporated into C?C triple bonds and diverse α-alkylated ketones were synthesized. Mechanism studies revealed that this reaction involves highly reactive alkyl free radicals. A unique equilibrium between lauric acid and water catalyzed by the iron(III) catalyst was observed.
- Zhu, Xiaotao,Ye, Changqing,Li, Yajun,Bao, Hongli
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supporting information
p. 10254 - 10258
(2017/08/07)
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- Iron-catalyzed C-H alkylation of heterocyclic C-H bonds
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An efficient, iron-catalyzed C-H alkylation of benzothiazoles by using alkyl diacyl peroxides and alkyl tertbutyl peresters which are readily accessible from carboxylic acids to synthesize 2-alkylbenzothiazoles is developed. This reaction is environmentally benign and compatible with a broad range of functional groups. Various primary, secondary, and tertiary alkyl groups can be efficiently incorporated into diverse benzothiazoles. The effectiveness of this method is illustrated by late-stage functionalization of biologically active heterocycles.
- Babu, Kaki Raveendra,Zhu, Nengbo,Bao, Hongli
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supporting information
p. 46 - 49
(2017/11/28)
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- Method for producing acyl peroxides
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The invention relates to a method for producing acyl peroxides. According to said method, an acyl compound is reacted with an organic hydroperoxide and a base, the pH of the two-phase mixture so obtained is adjusted to 6 to 13, the obtained organic phase is extracted with an aqueous solution of a base and the aqueous extract is recirculated to the reaction step. The method according to the invention allows the recirculation of unreacted hydroperoxide to the reaction step.
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Page/Page column 4
(2010/02/17)
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- Continuous Method for Producing Acyl Peroxides
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The invention relates to a continuous method for producing acyl peroxides. According to said method, an acyl chloride, carboxylic acid anhydride or chloroformate is reacted with an organic hydroperoxide or hydrogen peroxide in at least two mixed reaction zones that are connected in series, the acyl compound, the peroxy compound and an aqueous solution of a base being supplied to the first reaction zone. The first reaction zone comprises a cycle for the two-phase reaction mixture via a heat exchanger in which the reaction mixture is cooled. The method allows the reaction to be carried out reliably and with high space-time yields.
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Page/Page column 4
(2010/03/02)
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- METHOD FOR THE PRODUCTION OF ORGANIC PEROXIDES BY MEANS OF A MICROREACTION TECHNIQUE
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The invention provides a process for efficient and reliable preparation of organic peroxides, preferably dialkyl peroxides, peroxycarboxylic acids, peroxycarboxylic esters, diacyl peroxides, peroxycarbonate esters, peroxydicarbonates, ketone peroxides and perketals with the aid of at least one static micromixer and an apparatus for performing the process.
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Page/Page column 5
(2009/03/07)
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