Glycerol → HCID 78063027, compound

Temperature

72.5 °C

Separately, a 100 ml mixing vessel equipped with a calcium chloride-containing tube was charged with 36.9 g (0.20 mole) of 1,2-epoxydodecane. While the charged 1,2-epoxydodecane was stirred and cooled with water, a concentrated sulfuric acid was gradually dropped in an amount of 0.4 g (0.004 mole) into the cooled 1,2-epoxydodecane. After stirring for 15 minutes, the resultant mixture was placed into the dropping apparatus attached to the reaction vessel and was dropped into glycerol contained in the reaction vessel and maintained at a temperature of 70 to 75° C. over a time of 2 hours. Then the reaction of the mixture was carried out at a temperature of 70 to 75° C. for one hour. After the exhaustion of the starting material, namely 1,2-epoxydodecane, was confirmed by a thin-layer chromatography, the reaction was stopped. A powdered sodium hydrogen carbonate solution was mixed in an amount of 0.4 g (0.005 mole) into the resultant reaction liquid in the reaction vessel, the resultant mixture was stirred for 30 minutes to neutralize the reaction liquid. From the reaction liquid, precipitated crystals were separated by filtration. A glycerol monohydroxydodecyl ether mixture was obtained in an amount of 55.3 g (yield: 96.7%)

1. additionSeparately, a 100 ml mixing vessel
2. additioncontaining tube
3. customThen the reaction of the mixture
4. waitwas carried out at a temperature of 70 to 75° C. for one hour
5. customreaction liquid in the reaction vessel
6. customthe reaction liquid
7. customFrom the reaction liquid
8. customprecipitated crystals
9. customwere separated by filtration

ORD record

ord-9c62849937214294b487f0219dbd6011

Source dataset

uspto-grants-2006_11

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07138365B2