36768-62-4Relevant academic research and scientific papers
Catalyst-free method for synthesizing 2, 2, 6, 6-tetramethyl-4-piperidylamine
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Paragraph 0023-0039, (2021/05/01)
The invention provides a method for synthesizing 2, 2, 6, 6-tetramethyl-4-piperidylamine without a catalyst. Comprising the following steps: adding 2, 2, 6, 6-tetramethyl-4-piperidone and ammonium formate which is 1.25-1.6 times of the equivalent weight of the 2, 2, 6, 6-tetramethyl-4-piperidone into a reactor, and carrying out a Leuckart reaction, so as to obtain the 2, 2, 6, 6-tetramethyl-4-piperidylamine. According to the method, 2, 2, 6, 6-tetramethyl-4-piperidone and ammonium formate are adopted to react under the conditions of no catalyst, normal pressure or high pressure and no hydrogen; and the method provided by the invention has the advantages of high safety, high reaction selectivity, no generation of byproduct tetramethylpiperidinol, and effective increase of the yield. The method can be carried out without complex equipment, and is simple, convenient to operate, high in safety, high in repetition rate and low in cost.
2,2,6,6-tetramethyl-4-piperidinamine preparation method
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Paragraph 0024-0028, (2020/03/09)
The invention relates to a 2,2,6,6-tetramethyl-4-piperidinamine preparation method, which comprises: adding a raw material 2,2,6,6-tetramethylpiperidone, an amine reactant and a solvent into a reaction kettle, stirring and premixing at 10-50 DEG C to form an imine intermediate, reducing the imine intermediate by using a reducing agent at a certain temperature under a certain pressure, and reactingfor a certain time to finally synthesize the target product 2,2,6,6-tetramethyl-4-piperidinamine compound. According to the invention, 2,2,6,6-tetramethyl-4-carbonyl piperidone reacts with an amine compound to generate an imine intermediate, and a reducing agent is used for replacing catalytic hydrogenation to perform reduction, so the product yield can reach more than 92%, the generation of the2,2,6,6-tetramethylpiperidone hydrogenation byproduct tetramethylpiperidinol is avoided, the hydrogenation process with a high risk coefficient is avoided, and the method is an ideal process for achieving industrialization.
Synthetic method of amino-2,2,6,6-tetramentylniperidine with specific pH range
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Paragraph 0025; 0038-0073, (2019/07/04)
The invention discloses a synthetic method of amino-2,2,6,6-tetramentylniperidine with a specific pH range, and the method comprises the following steps: taking 2,2,6, 6-tetramethyl piperidone as a raw material, adding the raw material and ammonia water into a high-pressure kettle, first adjusting the pH value to 12.0-13.0, adding framework nickel serving as a catalyst, carrying out hydrogenationreaction at temperature of 55-65 DEG C under a set pressure value of 1.5-2.5 mpa, stopping the reaction until the pressure in the kettle is always not lower than 2% of a set pressure value in one hour; and carrying out normal pressure distillation on the reaction liquid, and then carrying out reduced pressure rectification to obtain the product amino-2,2,6,6-tetramentylniperidine. According to themethod disclosed by the invention, the conversion rate of the tetramethyl piperidone is improved, and the product yield is improved.
Method for preparing intermediate 2,2,6,6-tetramethyl-4-piperidylamine
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Paragraph 0039; 0042; 0044, (2019/12/25)
The invention relates to a method for preparing intermediate 2,2,6,6-tetramethyl-4-piperidylamine. The method is characterized by comprising the following steps: step 1), in the presence of a catalyst1, reacting acetone with ammonia gas to produce 2,2,6,6-tetramethyl-4-piperidinone and water; and step 2), in the presence of a catalyst 2, reacting the 2,2,6,6-tetramethyl-4-piperidinone with ammonia gas to produce 2,2,6,6-tetramethyl-4-piperidylimine and water, and reacting the 2,2,6,6-tetramethyl-4-piperidylimine with hydrogen gas to produce the 2,2,6,6-tetramethyl-4-piperidylamine, wherein the catalyst 1 is ammonium nitrate, and the catalyst 2 is a sodium hydroxyphenyl phosphate modified framework nickel catalyst. The method provided by the invention has the advantages of short synthetictime, a high conversion rate of the acetone and a high repeating utilization rate of the raw materials.
Synthesis and fluorescence properties of six fluorescein-nitroxide radical hybrid-compounds
Sato, Shingo,Endo, Susumu,Kurokawa, Yusuke,Yamaguchi, Masaki,Nagai, Akio,Ito, Tomohiro,Ogata, Tateaki
, p. 66 - 71 (2016/07/06)
Six fluorescein-nitroxide radical hybrid-compounds (2ab, 3ab, 4, and 5) were synthesized by the condensation of 5- or 6-carboxy-fluorescein and 4-amino-TEMPO (2ab), 5- or 6-aminofluorescein and 4-carboxy-TEMPO (3ab), and fluorescein and 4-carboxy-TEMPO (4), or by reaction of the 3-hydroxyl group of fluorescein with DPROXYL-3-ylmethyl methanesulfonate (5). Fluorescence intensities (around 520 nm) after reduction of the radical increased to 1.43-, 1.38-, and 1.61-folds for 2a, 2b and 3b respectively; 3a alone exhibited a decrease in intensity on reduction. Since 4 was readily solvolyzed in PBS or even methanol to afford fluorescein and 4-carboxy-TEMPO, its fluorescence change could not be measured. Hybrid compound 5 containing an ether-linkage between the fluorescein phenol and 3-hydroxymethyl-DPROXYL hydroxyl centers, was stable and on reduction, showed a maximum increase (3.21-fold) in relative fluorescence intensity in PBS (pH 5.0), despite its remarkably low absolute fluorescence intensity.
A 2, 2, 6, 6-tetramethyl-4-PIPERIDYLAMINES method for the preparation of
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Paragraph 0028; 0037-0042, (2017/04/11)
The invention discloses a method for preparing 2,2,6,6-tetramethyl-4-piperidinamine. The method comprises the following steps: synthesizing 2,2,6,6-tetramethyl-4-piperidone and carrying out a hydrogenation reaction of the 2,2,6,6-tetramethyl-4-piperidone. The key synthesis steps are controlled, the addition amount for acetone recovery is controlled, and the rectification purity and conversion rate of the product are improved through the optimized distillation, crystallization and hydrogenation reduction process.
MODIFIED ZNO NANOPARTICLES
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, (2012/05/04)
Process for the preparation of modified zinc oxide nanoparticles, which comprises reacting zinc oxide nanoparticles, which are dissolved in a solvent, in the presence of ammonia or amines with a tetraalkyl orthosilicate and optionally with an organosilane, with the proviso that the reaction takes place at a content of less than 5% by weight of water, based on the total amount of solvent and water. Modified zinc oxide nanoparticles which have Si—O-alkyl groups and are soluble in organic solvents, obtainable by this process for the preparation. Liquid or solid formulations which comprise modified ZnO nanoparticles. Inanimate organic materials, for example plastics or coatings, which comprise modified ZnO nanoparticles. Method of stabilizing inanimate organic materials against the effect of light, free radicals or heat, where modified ZnO nanoparticles, which optionally comprise UV absorbers and/or stabilizers as further additives, are added to the materials.
Reactions of nitroxides. Part X: Antifungal activity of selected sulfur and selenium derivatives of 2,2,6,6-tetramethylpiperidine
Zakrzewski, Jerzy,Krawczyk, Maria
scheme or table, p. 514 - 516 (2011/02/28)
The antifungal activity of nitroxyl radicals - derivatives of 2,2,6,6-tetramethylpiperidine-1-oxyl with reactive substituents 4-isothiocyanato-, 4-isocyano-, and 4-isoselenocyanato- and of N-formyl-, N-thioformyl-, N-selenoformyl-derivatives of 2,2,6,6-tetramethylpiperidine was investigated. Those of the above compounds, which contain a sulfur or selenium atom are the most active against four fungus plant patogens: Botrytis cinerea, Fusarium culmorum, Phytophthora cactorum, Rhizoctonia solani. 4-Isoselenocyanato-2,2,6,6-tetramethylpiperidine-1-oxyl proved to be the most active compound.
Electron paramagnetic resonance (EPR) study of spin-labeled camptothecin derivatives: A different look of the ternary complex
Ricci, Antonio,Marinello, Jessica,Bortolus, Marco,Sánchez, Albert,Grandas, Anna,Pedroso, Enrique,Pommier, Yves,Capranico, Giovanni,Maniero, Anna Lisa,Zagotto, Giuseppe
supporting information; experimental part, p. 1003 - 1009 (2011/04/25)
Camptothecin (CPT) derivatives are clinically effective poisons of DNA topoisomerase I (Top1) able to form a ternary complex with the Top1-DNA complex. The aim of this investigation was to examine the dynamic aspects of the ternary complex formation by means of site-directed spin labeling electron paramagnetic resonance (SDSL-EPR). Two semisynthetic CPT derivatives bearing the paramagnetic moiety were synthesized, and their biological activity was tested. A 22-mer DNA oligonucleotide sequence with high affinity cleavage site for Top1 was also synthesized. EPR experiments were carried out on modified CPT in the presence of DNA, of Top1, or of both. In the last case, a slow motion component in the EPR signal appeared, indicating the formation of the ternary complex. Deconvolution of the EPR spectrum allowed to obtain the relative drug amounts in the complex. It was also possible to demonstrate that the residence time of CPT "trapped" in the ternary complex is longer than hundreds of microseconds.
PROCESS FOR THE PREPARATION OF 4-AMINO-2,2,6,6-TETRAMETHYLPIPERIDINE
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Page/Page column 3-4, (2009/09/05)
4-amino-2,2,6,6-tetramethylpiperidine is prepared by reacting 2,2,6,6-tetramethylpiperidine-4-one with ammonia and hydrogen in the presence of nickel and/or cobalt catalyst and water. The main reaction is carried out at a pressure of at most 50 bar and a temperature of at most 120° C. up to a conversion of the 2,2,6,6-tetramethylpiperidine-4-one of at least 80%. Then, an after-reaction takes place at a higher temperature and at a higher pressure compared to the pressure and temperature of the main reaction.
