Epichlorohydrin → Diglycidyl ether

To a mixture of 382 g (4.13 moles) of epichlorohydrin and 86 g (0.21 mole) of bis(1,1,1,3,3,3-hexafluoro-2-hydroxyisopropyl)cyclohexane (Compound A) obtained in Reference Example 2 were added 16.8 g (0.42 mole) of sodium hydroxide and 2 ml of water. The mixture was heated with stirring and reacted with reflux for 10 hours. The resulting sodium chloride was removed by filtration with use of a glass filter and the excess of epichlorohydrin was distilled off at a reduced pressure. The residue was checked by gel permeation chromatography (GPC) to find that the compounds of the formula (1) in which n was 0, 1 and 2 were contained in 93:6:1 (ratio of area on chromatogram). Conditions for GPC: column, Shodex, KF-801, KF-802, each 30 cm, solvent, chloroform. The reside was distilled to obtain 50 g of diglycidyl ether of the compound of the formula (1) wherein n was zero, namely Compound A. The ether had a boiling point of 138° to 150° C./1 mmHg.

1. customobtained in Reference Example 2
2. temperatureThe mixture was heated
3. customreacted
4. temperaturewith reflux for 10 hours
5. customThe resulting sodium chloride was removed by filtration with use of a glass
6. filtrationfilter
7. distillationthe excess of epichlorohydrin was distilled off at a reduced pressure
8. distillationThe reside was distilled

ORD record

ord-40d63c9b7a6a47d2a9063d05bcf8f0fa

Source dataset

uspto-grants-1993_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05202360