Sodium Chloride → 2-{[4-(Ethenyloxy)butoxy]methyl}oxirane

Temperatur

40 °C

1,000 g (8.61 mol) of 4-hydroxybutyl vinyl ether (HBVE manufactured by Maruzen Petrochemical) and 448 g (11.2 mol) of sodium hydroxide were charged in a 3 L cylindrical flask equipped with a stirrer, a thermometer and a dropping funnel. The temperature was raised to 40° C. under stirring, 1,243 g (13.4 mol) of epichlorohydrin was then gradually added, and a reaction was conducted under controlling to 40° C. to 60° C. At after 8 hours of the reaction, the sodium chloride generated by the reaction was removed by filtration, 1,000 g of hexane was put therein, and the mixture was washed with 400 g of a 3% aqueous solution of sodium hydrogen sulfate and further washed with 800 g of 17% brine. The organic layer was concentrated by using a rotary evaporator to thereby distill the hexane off, and filtration was conducted to give the objective vinyloxybutyl glycidyl ether with a purity of 94% and a yield of 94%. At this time, the 4-hydroxybutyl vinyl ether contained in the obtained substance was 0.5%.

1. customequipped with a stirrer
2. customunder controlling to 40° C. to 60° C
3. customAt after 8 hours of the reaction
4. customwas removed by filtration, 1,000 g of hexane
5. washthe mixture was washed with 400 g of a 3% aqueous solution of sodium hydrogen sulfate
6. washfurther washed with 800 g of 17% brine
7. concentrationThe organic layer was concentrated
8. customa rotary evaporator
9. distillationto thereby distill the hexane off, and
10. filtrationfiltration

ORD-Eintrag

ord-e6da892f27704abca5013050b3564cb5

Quelldatensatz

uspto-grants-2016_07

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09394265B2