Hydrochloric Acid → 1--Dodecyl hydrogen oxybisacetate

HRID 851448

Reaktionsgleichung

Reaktionsgleichung von HRID 851448
[CH2:1]([OH:13])[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12].[O:14]1[C:19](=[O:20])[CH2:18][O:17][CH2:16][C:15]1=[O:21].Cl>N1C=CC=CC=1>[O:17]([CH2:18][C:19]([O:13][CH2:1][CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH3:12])=[O:20])[CH2:16][C:15]([OH:21])=[O:14]

Komponenten

5

Edukt 3

HCID 313Hydrochloric AcidHCID 81931-DodecanolHCID 782321,4-Dioxane-2,6-dione

Produkt 1

HCID 540892281--Dodecyl hydrogen oxybisacetate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 1049PyridineLösungsmittel

Versuchsvorschrift

18.6 g n-dodecanol was dissolved in 25 ml pyridine on a steam bath. When 11.6 g of 1,4-dioxane-2,6-dione was added with stirring, the mixture quickly reached 80° C. After 5 minutes the solution was allowed to cool to room temperature and, after 2 hours, was poured into 200 ml 1 N HCl. The gel which precipitated was extracted with 300 ml ether, washed three times, with 0.1 N HCl and dried over Na2SO4. The ether was evaporated and the resulting clear oil was taken up in petroleum ether. Agitation and cooling under nitrogen precipitated a product which was separated by filtration. The remaining solution was diluted to 250 ml with petroleum ether for precipitation of a second crop. The yield totalled 18.1 g of a white crystalline solid that melted at 57°-59° C. and was soluble in acetone, chloroform, ether and/or methanol. Elemental analysis indicated 56.8% C; 8.5% H (Calc. 56.7% C; 8.5% H).

Aufarbeitung

  1. customthe mixture quickly reached 80° C
  2. customThe gel which precipitated
  3. extractionwas extracted with 300 ml ether
  4. washwashed three times
  5. dry with materialwith 0.1 N HCl and dried over Na2SO4
  6. customThe ether was evaporated
  7. temperatureAgitation and cooling under nitrogen
  8. customprecipitated a product which
  9. customwas separated by filtration
  10. additionThe remaining solution was diluted to 250 ml with petroleum ether for precipitation of a second crop

Quellen und Nachweise

ORD-Eintrag
ord-cbb8bf3e570040b696ee7c9cceef77eb
Quelldatensatz
uspto-grants-1983_05
Patentnummer
US04384969

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