CS209332B1 - Preparation method of /1-methyldodecyl/-dimethylamine - Google Patents
Preparation method of /1-methyldodecyl/-dimethylamine Download PDFInfo
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- CS209332B1 CS209332B1 CS805478A CS547880A CS209332B1 CS 209332 B1 CS209332 B1 CS 209332B1 CS 805478 A CS805478 A CS 805478A CS 547880 A CS547880 A CS 547880A CS 209332 B1 CS209332 B1 CS 209332B1
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- dimethylamine
- methyldodecyl
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Abstract
SpSaob přípravy /1-metyldodecyl/dimetylemínu Organická chémia Syntéza Syntéza /1-metyldodecyl/dimetylamínu z 2-tridekanónu pomocou dimetylamínu a vodíka na Řaney-nikli a za tlaku 8 MPa. finálny produkt slúži ako medziprodukt pri príprave biologicky účinných, látok. Chemický priemysel, kozmetika, farmaceutický priemysel, vláknársky priemysel.Preparation of (1-methyldodecyl) dimethylemine Organic Chemistry Synthesis Synthesis of (1-methyldodecyl) dimethylamine from 2-tridecanone with dimethylamine and hydrogen on Raney-nickel and under pressure 8 MPa. the final product serves as an intermediate biologically active substances. Chemical industry, cosmetics, pharmaceutical industry, the fibrous industry.
Description
Vynález sa týká spósobu přípravy /l-metyldodecyl/dimetylamínu vzoroa CH3 - OH - /0H2/10 - CH3 GH3 - N - CttjBACKGROUND OF THE INVENTION The present invention relates to a process for the preparation of (1-methyldodecyl) dimethylamine and CH3 - OH - / 0H2 / 10 - CH3 GH3 - N - Ctt3
Niektoré deriváty 1-metyldodecylamínu /starší néssov 2-aminotridekán/ sa v súčaenosti používajú ako antimikrobiálne účinné' zlúčeniny. Sú to zlúčeniny odvedené teda od pri- márného aminu. Niektoré dalšie deriváty /napr. amoniové soli, amínoxidy/ ai však vyžadujú ako výohodiskovú surovinu terciámy amin, sajlepšie /1-metyldodecyl/dimetylamín. Teroiárny amin takéhoto typu je možné připravit niekolkými metodami, napr. alkyláoiou primárného aminu šlkylačnými šinidlami typu dimetylaulfátu alebo jódmetánu, alebo reakoiou 2-halo- génalkánov a dimetylamínom. Všetký tieto procesy vedú však k produktem nízkej čistoty a výtažky aú taktiež neuspokojivé.Some 1-methyldodecylamine derivatives / older n-2-aminotridecanes are also used as antimicrobial active compounds. Thus, they are compounds removed from the primary amine. Some other derivatives / e.g. however, ammonium salts, amine oxides, and the like require a tertiary amine, the best 1-methyldodecyl / dimethylamine, as the feedstock. A tertiary amine of this type can be prepared by several methods, e.g. However, all these processes lead to low purity products and extracts are also unsatisfactory.
Uvedené nevýhody odstraňuje spósob přípravy /1-metyldodeoyl/dimetylamínu horeuvedeného vzoroa, ktorého podstatou je, že sa neohá zreagovat 2-tridekanón vzoroa 0H3 - C - /CHg/io ~ CH3 0 a dimetylamínom v atmosféře vodíka pri tlaku 8 MPa a teplote 100 ®C v prostředí metanolu za katalýzy Raney-niklom po dobu 3,5 h. Týmto spósobom vzniká takmer v kťantitatívnom výtažku /1-metyldodeoyl/dimetylamín. Táto metoda má tú výhodu, že v porovnaní s metodami uvedenými v literatúre poskytuje takmer kvantitativné výtažky. Napr. Org. Raaotionsé, 174 /1949/ udává, že reakcia alifatických ketónov s dimetylamínom za přítomnosti katalyzátore a vodíka u ketónov a dlhším reťazoom ako so síedmimi uhlíkmi /2-heptahón/ neprabiaha, alebo prebieha len v nepatrných výtažkoch. Sálej uvedený příklad ilustruje spósob přípravy podlá vynálezu. PříkladThe above drawbacks are overcome by the method of preparing 1-methyldodeoyl / dimethylamine of the above formula, which is based on the fact that 2-tridecanone of the formula and OH3-C- (CH3) 10 -CH3 O and dimethylamine cannot be reacted under a hydrogen atmosphere at 8 MPa and 100 DEG C. C in Raney-nickel catalysis with methanol for 3.5 h. In this way almost 1-methyldodeoyl / dimethylamine is obtained in almost quantitative yield. This method has the advantage that it provides almost quantitative extracts compared to the methods disclosed in the literature. E.g. Org. Raaotions, 174 (1949) reports that the reaction of aliphatic ketones with dimethylamine in the presence of a catalyst and hydrogen in ketones and a longer chain than in the case of the eight carbon (2-heptahone) does not occur, or occurs only in small amounts. The example below illustrates the method of the invention. Example
Do vodíkem prepláohnutého autoklávu sa dá 1,5 mol 2-tridekanónu, 35 g Raney-aiklu, 4mol dime tylamínu. a 500 ml metanolu. Po uzavretí sa tlak v autokláve upraví vodíkom na 8 MPa a reakčná zmes za zahraje na 100 °C. Po 1,5 h sa absorbuje vypočítané množstvo vodíka, reakčná zaea sa neohá doreagovat dalšie 2 h. Po ochladení sa Raney-nlkel odfiltruje, metanol sa odpaří a produkt aa predestiluje. T.v. 156 až 158 °0 /2,7 až 3 kPaj n§° 1,4440, výtažek 90 % hmot., l8 - spektrálná charakteristika» V /N-OHj/ 2767 om"·1, (O/CHg/ 711 om"1.1.5 mol of 2-tridecanone, 35 g of Raneylic, 4 mol of dimethylamine are added to the hydrogen-purged autoclave. and 500 ml of methanol. After closing, the pressure in the autoclave is adjusted to 8 MPa with hydrogen and the reaction mixture is heated to 100 ° C. After 1.5 h, the calculated amount of hydrogen is absorbed, and the reaction is not allowed to react for another 2 h. After cooling, Raneylkel is filtered off, the methanol evaporated and the product distilled. T.v. 156 to 158 ° 0 / 2.7 to 3 kPaj n§ ° 1.4440, 90% mass extract, 18 - spectral characteristic »V / N-OHj / 2767 om" · 1, (O / CHg / 711 om ") 1.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS805478A CS209332B1 (en) | 1979-06-20 | 1980-08-08 | Preparation method of /1-methyldodecyl/-dimethylamine |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CS423979A CS205187B1 (en) | 1979-06-20 | 1979-06-20 | Manufacturing method of thermal-insulating material with antifire effects |
| CS805478A CS209332B1 (en) | 1979-06-20 | 1980-08-08 | Preparation method of /1-methyldodecyl/-dimethylamine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CS209332B1 true CS209332B1 (en) | 1981-11-30 |
Family
ID=5384668
Family Applications (2)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS423979A CS205187B1 (en) | 1979-06-20 | 1979-06-20 | Manufacturing method of thermal-insulating material with antifire effects |
| CS805478A CS209332B1 (en) | 1979-06-20 | 1980-08-08 | Preparation method of /1-methyldodecyl/-dimethylamine |
Family Applications Before (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CS423979A CS205187B1 (en) | 1979-06-20 | 1979-06-20 | Manufacturing method of thermal-insulating material with antifire effects |
Country Status (1)
| Country | Link |
|---|---|
| CS (2) | CS205187B1 (en) |
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1979
- 1979-06-20 CS CS423979A patent/CS205187B1/en unknown
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1980
- 1980-08-08 CS CS805478A patent/CS209332B1/en unknown
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| Publication number | Publication date |
|---|---|
| CS205187B1 (en) | 1981-05-29 |
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