Glycerol → HCID 86708448、化合物

温度

120 °C

A stirred autoclave was charged, at room temperature, with 66.75 g (725 mmol) of glycerol, 2.05 g (17.6 mmol) of caproic acid, 0.20 g (10 wt %) of AMBERLYST® (a polymer based catalyst) 35 resin and 0.39 g (1.0 mol %) of Pd/C at 5%. The autoclave was then pressurized at 50 bar of dihydrogen gas H2, and then it was heated at 120° C. for 16 h, stirring vigorously. After 16 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 purified on a flash silica column (eluent:cyclohexane/ethyl acetate=4:1˜1:1). 1-O-hexyl-glycerol ether was obtained at an isolated yield of 70%.

1. customAfter 16 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
12. customwas purified on a flash silica column (eluent:cyclohexane/ethyl acetate=4:1˜1:1)

ORDレコード

ord-e85f1a1218af47dc9b71b2aff7489632

出典データセット

uspto-grants-2014_12

DOI

10.6084/m9.figshare.5104873.v1

特許番号

US08912365B2