Sorbitol → Hexitolato--oxiranato (1/1)

Temperature

130 °C

Sorbitol (Wako Pure Chemical Industries, Ltd., 250 g, hereinafter, also referred to as “SB”) and a 30% sodium hydroxide aqueous solution (3.44 g) were charged into a pressure-resistant reaction vessel equipped with a stirrer. The temperature of the reaction system was heated to 130° C. with an oil bath. The pressure of the reaction system was reduced to 100 mmTorr for 1 hour with a vacuum pump while nitrogen was slowly bubbled into the reaction system, and thereby water was distilled off. The pressure was further kept at 100 mmTorr for 1 hour with a vacuum pump. Then, the inner pressure was adjusted to 0.5 MPa by nitrogen introduction. While the inner temperature was kept at 130° C.±2° C., ethylene oxide (1,813.6 g, 30-fold mole relative to SB) was added. The inner pressure was controlled so as not to exceed 0.8 MPa. After the ethylene oxide addition, the inner temperature was kept at 130° C. for 1 hour to complete the reaction. The yield was found to be 99.7% from the masses before and after the reaction. The reaction provided a sorbitol ethylene oxide 29.9 mol adduct (hereinafter, also referred to as “SB-30”).

1. additionwere charged into a pressure-resistant reaction vessel
2. customequipped with a stirrer
3. customwas slowly bubbled into the reaction system
4. distillationwater was distilled off
5. waitThe pressure was further kept at 100 mmTorr for 1 hour with a vacuum pump
6. customwas kept at 130° C.±2° C.
7. additionethylene oxide (1,813.6 g, 30-fold mole relative to SB) was added
8. additionAfter the ethylene oxide addition
9. waitthe inner temperature was kept at 130° C. for 1 hour
10. customthe reaction
11. customafter the reaction

ORD record

ord-fa78ecb943ac4a1a84dd9e9d304580d2

Source dataset

uspto-grants-2013_07

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08476341B2