CS252977B1 - Hydrogen sulphate of 2,2,6,6-tetramethyl-4,4-piperidinium acetic acid and method of its preparation - Google Patents

Hydrogen sulphate of 2,2,6,6-tetramethyl-4,4-piperidinium acetic acid and method of its preparation Download PDF

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Publication number
CS252977B1
CS252977B1 CS859499A CS949985A CS252977B1 CS 252977 B1 CS252977 B1 CS 252977B1 CS 859499 A CS859499 A CS 859499A CS 949985 A CS949985 A CS 949985A CS 252977 B1 CS252977 B1 CS 252977B1
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CS
Czechoslovakia
Prior art keywords
tetramethyl
piperidinium
preparation
acetic acid
hydrogen sulphate
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Application number
CS859499A
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Czech (cs)
Slovak (sk)
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CS949985A1 (en
Inventor
Frantisek Vass
Anna Bielikova
Zdenek Manasek
Jozef Luston
Gabriela Vassova
Original Assignee
Frantisek Vass
Anna Bielikova
Zdenek Manasek
Jozef Luston
Gabriela Vassova
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Application filed by Frantisek Vass, Anna Bielikova, Zdenek Manasek, Jozef Luston, Gabriela Vassova filed Critical Frantisek Vass
Priority to CS859499A priority Critical patent/CS252977B1/en
Publication of CS949985A1 publication Critical patent/CS949985A1/en
Publication of CS252977B1 publication Critical patent/CS252977B1/en

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  • Heterocyclic Carbon Compounds Containing A Hetero Ring Having Oxygen Or Sulfur (AREA)
  • Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)

Description

Stéricky bráněné aminy sú v porovnaní s klasickými UV-absorbérmi mimoriadne účinné světelné stabilizátory polymérov. Inhibujú nežiadúce radikálové procesy, ktoré sprevádzajú fotooxidačnú degradáciu polymérov, najma polyolefínov. Nevýhodou mnohých zlúčenín tejto skupiny je ich značná prchavosť, vykvétanie a extrahovatelnosť z polymérnych materiálov. Riešenie týchto problémov poskytuje zvyšovanie molekulovej hmotnosti týchto stabilizátorov, alebo naviazanie účinného skeletu na hlavný reťazec úžitkového polyméru. V literatúre doslal' nie je známa zlúčenina, ktorá je predmetom vynálezu. Podstatou vynálezu je hydrogénsíran kyseliny 2,2,6,6-tetrametyl-4-piperidíniumdioctovej vzorca ISterically hindered amines are particularly effective light stabilizers of polymers compared to conventional UV absorbers. They inhibit undesirable radical processes that accompany photooxidative degradation of polymers, especially polyolefins. A disadvantage of many compounds of this group is their high volatility, flowering and extractability from polymeric materials. A solution to these problems is provided by increasing the molecular weight of these stabilizers, or by attaching an effective backbone to the backbone of the useful polymer. The compound of the present invention is not known in the literature. The present invention provides 2,2,6,6-tetramethyl-4-piperidinium di-acetic acid bisulfate

Predmetnú látku možno připravit tak, že sa na amóniovú sol' l,5-dikyano-3,4-dioxo-8,8,10,10-tetrametyl-3,9-diazaspiro [ 5,5 ] undekánu vzorca IIThe subject compound can be prepared by treating the ammonium salt of 1,5-dicyano-3,4-dioxo-8,8,10,10-tetramethyl-3,9-diazaspiro [5,5] undecane of formula II

O, ho''· h3c CH<0, ho &quot; h 3 c CH <

CH~CH ~

OHOH

HSQ$ (DHSQ $ (D

NCNC

H3CH 3 C

H^CH + C

C CC C

J-CN pósobí koncentrovanou kyselinou sírovou a potom sa k reakčnej zmesi přidá destilovaná voda a reakčná zmes sa zahrieva po dobu 6 až 10 h pri teplote 80 až 100 °C.The J-CN is treated with concentrated sulfuric acid, then distilled water is added to the reaction mixture, and the reaction mixture is heated at 80 to 100 ° C for 6-10 h.

Uvedená látka má využitie na přípravu polymérnych světelných stabilizátorov polyesterového typu so zníženou extrahovatel'nosťou z polymérov.Said substance is used for the preparation of polyester type light stabilizers with reduced extractability from polymers.

Příklad 1Example 1

K 1,53 g (0,005 molu) amóniovej soli 1,5252977To 1.53 g (0.005 mol) of the ammonium salt 1.5252977

-dikyano-2,4-dioxo-8,8,10,10-tetrametyl-3,9-diazaspiro'[5,5]undekánu sa přidá 1,5 mililitra koncentrované] kyseliny sírové], zmes sa opatrné zahrieva, pričom systém nadobúda viskóznu konzistenciu. Po štátí réakčne] zmesi cez noc sa na druhý deň k nej přidá 2 ml destilovanej vody a roztok sa nechá zahrievať pri teplote 80 °C po dobu 10 hodin. Z reakčnej zmesi sa počas tejto doby uvolňuje reakčný oxid uhličitý. Po ochladení na 15 °C z roztoku kryštalizuje produkt v podobě bezfarebných priehladných kryštálkov, ktoré sa odsajú a premyjú malým množstvom studenej destilované] vody. Získá sa 1,52 g produktu (85,9%) s teplotou topenia 217 až 220 °C.-dicyano-2,4-dioxo-8,8,10,10-tetramethyl-3,9-diazaspiro [5.5] undecane is added 1.5 ml of concentrated] sulfuric acid], the mixture is heated gently while the system is heated. it has a viscous consistency. After standing overnight, 2 ml of distilled water was added thereto the next day and the solution was allowed to warm to 80 ° C for 10 hours. During this time, the reaction carbon dioxide is released from the reaction mixture. After cooling to 15 ° C from the solution, the product crystallizes as colorless transparent crystals, which are aspirated and washed with a small amount of cold distilled water. 1.52 g of product (85.9%) with a melting point of 217-220 ° C are obtained.

Elementárna analýza pre CisHzsNOsS Vypočítané:Elemental Analysis for C 18 H 18 NO 3 S Calculated:

C = 43,93 %, H = 7,09%, N = 3,94%C = 43.93%, H = 7.09%, N = 3.94%

Claims (2)

PREDMETSUBJECT 1. Hydrogénsíran kyseliny 2,2,6,6-tetrametyl-4,4-piperidíniumdioctovej vzorca I1. 2,2,6,6-Tetramethyl-4,4-piperidinium di-acetic acid hydrogen sulphate Nájdené:found: C = 44,25 %, H = 6,79 %, N = 3,54 % IČ spektrum (nujol):C = 44.25%, H = 6.79%, N = 3.54% IR (nujol): 3 620, 3 310, 2 940, 2 830, 2 700, 1740,3,620, 3,310, 2,940, 2,830, 2,700, 1740, 1 465, 1 375, 1 360 cm'1 Příklad 21 465, 1 375, 1 360 cm -1 Example 2 Postupovalo sa ako v příklade 1 s tým rozdielom, že sa reakcia robila pri teplote 100 °C po dobu 6 h.The procedure was as in Example 1 except that the reaction was carried out at 100 ° C for 6 h. Vynález má využitie v chémii polymérov, umožňuje přípravu polymérnych světelných stabilizátorov polykondenzačnými reakciami s diolmi.The invention has applications in polymer chemistry, allows the preparation of polymeric light stabilizers by polycondensation reactions with diols. ynAlezuINVENTION It -dioxo-8,8,10,10-tetrametyl-3,9-diazaspiro[5,5]undekánu vzorca II fa \ {i /-dioxo-8,8,10,10-tetramethyl-3,9-diazaspiro [5,5] undecane of formula II 2. Sposob přípravy hydrogénsíranu kyseliny 2,2,6,6-tetrametyl-4,4-piperidíniumdioctovej vzorca I pódia bodu 1, vyznačujúci sa tým, že sa na amóniovú sol' l,5-dikyano-2,4posobí koncentrovanou kyselinou sírovou a potom sak reakčnej zmesi přidá destilovaná voda a reakčná zmes sa zahrieva po dobu 6 až 10 h pri teplote 80 až 100 °C.2. A process for the preparation of 2,2,6,6-tetramethyl-4,4-piperidinium di-acetic acid hydrogen sulphate of the formula I as defined in claim 1, characterized in that it is treated with concentrated sulfuric acid on the 1,5-dicyano-2,4-ammonium salt and distilled water is then added to the reaction mixture and the reaction mixture is heated at 80 to 100 ° C for 6 to 10 h.
CS859499A 1985-12-19 1985-12-19 Hydrogen sulphate of 2,2,6,6-tetramethyl-4,4-piperidinium acetic acid and method of its preparation CS252977B1 (en)

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CS859499A CS252977B1 (en) 1985-12-19 1985-12-19 Hydrogen sulphate of 2,2,6,6-tetramethyl-4,4-piperidinium acetic acid and method of its preparation

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CS859499A CS252977B1 (en) 1985-12-19 1985-12-19 Hydrogen sulphate of 2,2,6,6-tetramethyl-4,4-piperidinium acetic acid and method of its preparation

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CS252977B1 true CS252977B1 (en) 1987-10-15

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