Glycerol → HCID 86708448, Verbindung

Temperatur

140 °C

A stirred autoclave was charged, at room temperature, with 55.2 g (600 mmol) of glycerol, 3.9 g (30 mmol) of methyl caproate, 0.4 g (10 wt %) of camphosulfonic acid and 0.3 g (0.5 mol %) of Pd/C at 5%. The autoclave was then pressurized at 30 bar of dihydrogen gas H2, and then it was heated at 140° C. for 24 h, stirring vigorously. After 24 h of reaction, the reaction mixture was brought back to room temperature. The catalyst was then filtered on a MILLIPORE® filter (a membrane filter)(0.45 μm) and was rinsed with absolute ethanol. The solvents were then evaporated and the organic products were extracted from the glycerol phase by extraction with CH2Cl2 (3×50 ml). The organic phase was washed with water (2×20 ml) and the CH2Cl2 was then evaporated at reduced pressure. The crude reaction product was analyzed by GC/MS. 1-O-hexyl-glycerol ether was obtained at 50% GC yield.

1. customAfter 24 h of reaction
2. customwas brought back to room temperature
3. filtrationThe catalyst was then filtered on a MILLIPORE®
4. filtrationfilter (a membrane
5. filtrationfilter)(0.45 μm)
6. washwas rinsed with absolute ethanol
7. customThe solvents were then evaporated
8. extractionthe organic products were extracted from the glycerol phase by extraction with CH2Cl2 (3×50 ml)
9. washThe organic phase was washed with water (2×20 ml)
10. customthe CH2Cl2 was then evaporated at reduced pressure
11. customThe crude reaction product

ORD-Eintrag

ord-a643dcac51ad48f0b6e836f2cf1b5ef0

Quelldatensatz

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US08912365B2