Glycerol → HCID 86708448、化合物

温度

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 40 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 55% 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レコード

ord-6157d9c652f74c3d824928a5dfdaba77

出典データセット

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08912365B2