CS215932B1 - 15- / 2,3-dihydroxypropyl / -7,15-diazadispiro 2? 1? - Google Patents

15- / 2,3-dihydroxypropyl / -7,15-diazadispiro 2? 1? Download PDF

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Publication number
CS215932B1
CS215932B1 CS345880A CS345880A CS215932B1 CS 215932 B1 CS215932 B1 CS 215932B1 CS 345880 A CS345880 A CS 345880A CS 345880 A CS345880 A CS 345880A CS 215932 B1 CS215932 B1 CS 215932B1
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Czechoslovakia
Prior art keywords
diazadispiro
dione
hexadecane
dihydroxypropyl
preparation
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CS345880A
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Czech (cs)
Slovak (sk)
Inventor
Frantisek Vass
Zdenek Manasek
Jozef Luston
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Frantisek Vass
Zdenek Manasek
Jozef Luston
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Application filed by Frantisek Vass, Zdenek Manasek, Jozef Luston filed Critical Frantisek Vass
Priority to CS345880A priority Critical patent/CS215932B1/en
Publication of CS215932B1 publication Critical patent/CS215932B1/en

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  • Nitrogen And Oxygen Or Sulfur-Condensed Heterocyclic Ring Systems (AREA)

Abstract

Vynález sa týká 15-/2,3-dihydroxypropyl/-7,15-diazadispiro-/JJ,1,5,27 hexadekán-14,l6-diónu a sposobu jeho pripravy. Podstata sposobu pripravy predmetnej zlúčeniny spočívá v tom, že na sodnú alebo draselnú sol 7,15-diazadispiro 1*5,27 hexadekán-14,16-diónu sa pfrsobí 1-chlor- -2,3-dihydroxypropánom. Látka připravená podlfe vynálezu má použitie ako světelný stabilizátor polymérov.The invention relates to 15-/2,3-dihydroxypropyl/-7,15-diazadispiro-/JJ,1,5,27 hexadecane-14,16-dione and a method for its preparation. The essence of the method for the preparation of the subject compound lies in the fact that the sodium or potassium salt of 7,15-diazadispiro 1*5,27 hexadecane-14,16-dione is reacted with 1-chloro- -2,3-dihydroxypropane. The substance prepared according to the invention has application as a light stabilizer of polymers.

Description

215 932 1

Vynález sa týká 15-/2,3-dihydroxypropyl/-7,15-diazadispiro /í>,1,5,27 hexadekán-14,16--diónu nasledujúceho vzoroaí

a sposobu jeho přípravy.

SpSsob přípravy zlúčeniny, ktorá nie je známa z literatúry, je založený na reakoll1-ehlór-2,3-dihydroxypropánu a 7,15-diazadispiro /5,1,5,27 bexadekán-14,16-diónom.

Uvedená zlúčenina patriaoa do skupiny stéricky bráněných amínov máze samotná pdsobiVako světelný stabilizátor polymérov. Nevýhodou nízkomolekulových zlúčenín tejto skupiny jeioh značná prohavosť a vypieratePnosť z úžitkového polyméru. Přípravou polymérnýoh světel-ných stabilizátorov sa tieto nedostatky dajú odstránit*. K tomuto účelu može slúžitf látka,ktorá je predmetom vynálezu. Přikladl 1 K 2,88 g (0,01 molu) draselnej soli 7,15-diazadispiro-/5’,1,5,27 hexadekán-14,16-diónuv 30 ml bezvodnáho dimetylformamidu sa za stálého miešania pri teplote okolo 80 °C prikvapkáva v priebehu 1/2 až 1 hodiny roztok 1,11 g (0,01 molu) 1-chlór-2,3-dihydroxypropánuv 15 ml bezvodáho dimetylformamidu. Zmes sa dblej zahrieva a mieša po dobu 3 hodin a ne-chá sa ochladit*. Vyextrahuje sa trikrát áterom a spojená áterioká extrakty sa dokladnépřemyjú vodou, vysušia bezvodým síranom sodným a éter sa odpaří. Obdržaný zvyšok sa pře-čistí chromátografioky. Získá sa produkt v podobě bielej kryštalickej látky s t.t. 70 -- 73 °C.

Blementárna analýza pre C^HggNgO^s

Vypočítané: C 62,94 H » 8,70 ΪΓ = 8,63 Nájdené: C 62,63 %» H · 8,67 N - 8,71 IČ spektrum (OHCl^): 980, 1020, 1035, 1070, 1120, 1160, 1190, 1265, max.a 1285, 1340, 1450, 1665, 1710, 2940, 3460 Příklad 2 100 hmotnostných dielov nestabilizovaného práškovitého polypropylénu sa impregnovalov dichlórmetáne s 0,1 hmot. dielmi 2,6-di-terc. butyl-4-metylfenolu, 0,15 hmot. dielmistearanu vápenatého a s 0,2 hmot. dielmi zlúčeniny, pripravenej podl*a příkladu 1. Po od-paření rozpúštfedla sa zo zmesi vylisovali fólie o hrúbke 0,2 mm pri tlaku 20 MPa a teplo-te 190 °C po dobu 30 sekúnd. Tesne před lisováním sa vzorky ešte-predohrieveli 1 minútupri teplote 190 °C. Folie sa očarovali ortutfovou výbojkou o výkone 125 W vo vzdialenosti7 cm od zdroje a ako filter sa použil 1,6 hmot. % roztok síranu medhatéhó. Degradácia po-

215 932 1

The invention relates to 15- (2,3-dihydroxypropyl) -7,15-diazadispiro [1,5] hexadecane-14,16-dione of the following formula

and the method of its preparation.

The method for the preparation of a compound which is not known in the literature is based on reacol1-chloro-2,3-dihydroxypropane and 7,15-diazadispiro (5,1,5,27 bexadecane-14,16-dione).

Said compound belonging to the group of sterically hindered amines melt itself acts as a light stabilizer of polymers. A disadvantage of the low molecular weight compounds of this group is the considerable creep and washability of the useful polymer. These drawbacks can be eliminated by preparing the polymeric light stabilizers. The substance of the invention may be used for this purpose. EXAMPLE 1 1 To 2.88 g (0.01 mole) of 7,15-diazadispiro- (5 ', 1,5,27) hexadecane-14,16-dione potassium salt in 30 ml of anhydrous dimethylformamide at about 80 ° with stirring C was added dropwise over 1 to 1 hour to a solution of 1.11 g (0.01 mol) of 1-chloro-2,3-dihydroxypropane in 15 ml of anhydrous dimethylformamide. The mixture was heated and stirred for 3 hours and was not allowed to cool. It is extracted three times with ether and the combined ether extracts are washed with water, dried over anhydrous sodium sulfate and the ether is evaporated. The residue obtained is purified by chromatography. The product was obtained as a white crystalline solid, mp 70-73 ° C.

Blement Analysis for C ^ HggNgO ^ s

Calcd. For C, 62.94; H, 8.70; C, 8.63; Found: C, 62.63;% H, 8.67; N, 8.71; IR (OHCl ^): 980, 1020, 1035, 1070, 1120. , 1160, 1190, 1265, max. 1285, 1340, 1450, 1665, 1710, 2940, 3460 Example 2 100 parts by weight of unstabilized polypropylene powder were impregnated with 0.1% by weight of dichloromethane. 2,6-di-tert. butyl 4-methylphenol, 0.15 wt. Calcium Diluate and 0.2 wt. of the compound prepared according to Example 1. After evaporation of the solvent, sheets of 0.2 mm thickness were pressed from the mixture at a pressure of 20 MPa and a temperature of 190 ° C for 30 seconds. Just before pressing, the samples were pre-heated for 1 minute at 190 ° C. The films were enchanted with a 125 W mercury discharge lamp at a distance of 7 cm from the source and 1.6 wt. % medhate sulfate solution. Degradation

Claims (2)

2 215 932 lyméru sa sledovala vývojom hydroperoxidového a karbonylového pásu v infračervených spektrach. Kým doba dosiahnutia karbonylového indexu 0,2 u čistého polypropylénu bola 4Θ0 ho-din, stabilizovaný polymer nedosiahol tuto hodnotu ani za 3000 hodin. PREDMET VYNÁLEZU 1. 15-/2,3-dihydroxypropyl/-7,15-diazadispiro ,5,27-hexadekán-14,l6-dión vzorca:The 2,215,932 polymer was monitored by developing a hydroperoxide and carbonyl band in infrared spectra. While the carbonyl index time of 0.2 for pure polypropylene was 40%, the stabilized polymer did not reach this value even after 3000 hours. OBJECT OF THE INVENTION 1. 15- / 2,3-Dihydroxypropyl / -7,15-diazadispiro, 5,27-hexadecane-14,16-dione of formula: 2. Sposob přípravy 15-/2»3-dihydroxypropyl/-7,15-diazadispiro ^,1,5,27 heXadekán--14,16-diónu podlít bodu 1, vyznačujúci sa tým, že na draselná alebo sodná sol’ 7,15-diaza-dispiro 1»5,27 hexadekán-14»l6-diónu sa posobí 1-chlór-2,3-dihydroxy-propánom.2. A process for the preparation of 15- (2,3-dihydroxypropyl) -7,15-diazadispiro, 1,5,27 hexadecane-14,16-dione according to claim 1, characterized in that the potassium or sodium salt is 15-diaza-dispiro-1,25-hexadecane-14,16-dione was introduced with 1-chloro-2,3-dihydroxy-propane.
CS345880A 1980-05-19 1980-05-19 15- / 2,3-dihydroxypropyl / -7,15-diazadispiro 2? 1? CS215932B1 (en)

Priority Applications (1)

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Applications Claiming Priority (1)

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