Hydrochloric Acid → 1--Dodecyl hydrogen oxybisacetate

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).

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

ORDレコード

ord-cbb8bf3e570040b696ee7c9cceef77eb

出典データセット

uspto-grants-1983_05

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US04384969