Acetic Acid → Octyl-sepharose CL-4B

온도

200 °C

In a reactor, 390 g of octanol, 2 g of aluminum triisopropoxide and 1.4 g of sulfuric acid were charged. After heating to 100° C., dehydration was conducted under reduced pressure (2.67 kPa). The residue was then cooled to 85° C., followed by the dropwise addition of 185 g of epichlorohydrin at a temperature maintained at 85° C. After stirring at 85° C. for 4 hours, an excess alcohol was removed at 100° C. under reduced pressure (0.67 kPa). To the crude octyl halohydrin ether thus obtained, 480 g of a 209 aqueous solution of sodium hydroxide was added and the resulting mixture was reacted at 90° C. for 2 hours. After completion of the reaction, the water layer was removed, whereby 315 g of crude octyl glycidyl ether was obtained. In an autoclave, 200 g of the resulting crude octyl glycidyl ether, 35 g of water, 11.8 g of 99% acetic acid and 12.1 g of a 48% aqueous solution of sodium hydroxide were charged, followed by stirring at 200° C. for 1 hour. At a temperature maintained at 200° C., 27.5 g of a 48% aqueous solution of sodium hydroxide was added dropwise over 3 hours and reaction was conducted for 1 hour. The reaction mixture was cooled to 80° C. While maintaining the temperature at 80° C., 150 g of water was added and the resulting mixture was stirred vigorously. The reaction mixture was allowed to stand to cause separation, followed by removal of the water layer. The operation from the addition of 150 g of water to the separation was then repeated three times. The reaction mixture was dehydrated at 100° C. under reduced pressure (5.32 kPa), whereby 224 g of monooctyl glyceryl ether was obtained. As a result of GLC, it was found that the resulting product had a purity of 91% and the content of organochlorine compounds was not greater than 100 ppm.

1. temperatureAt a temperature maintained at 200° C.
2. customreaction
3. waitwas conducted for 1 hour
4. temperatureThe reaction mixture was cooled to 80° C
5. temperatureWhile maintaining the temperature at 80° C.
6. stirringthe resulting mixture was stirred vigorously
7. customseparation
8. customfollowed by removal of the water layer
9. additionThe operation from the addition of 150 g of water
10. customto the separation
11. customwas dehydrated at 100° C. under reduced pressure (5.32 kPa)

ORD 기록

ord-046e808b62c1417bb530ac1e32d665e3

출처 데이터셋

uspto-grants-2002_08

DOI

10.6084/m9.figshare.5104873.v1

특허 번호

US06437196B1