Dichloromethane → 2-Ethoxyethyl triflate

Temperature

-5 °C

25 g of ethoxyethanol was placed in a round bottom flask provided with a stirrer piece therein, which was connected to a nitrogen bubbler to replace the air in the flask by dry nitrogen. 141 ml of methylene chloride was added and 33 ml of 2,6-lutidine was further added, followed by cooling down to −10 to 0° C., dropping 57 ml of trifluoromethanesulfonic acid anhydride in one hour and continuing agitation under the cooling conditions for one hour. 100 ml of distilled water was added to the reaction solution, and an organic phase was separated, washed with 100 ml of distilled water and dried with anhydrous sodium sulfate, followed by removing the sodium sulfate by filtration and distilling off the solvent under reduced pressure. The resulting residue was distilled under a reduced pressure of 150 Pa at 30° C. to obtain 57 g of a 2-ethoxyethyl triflate fraction.

1. customprovided with a stirrer piece
2. customin one hour
3. customfor one hour
4. customan organic phase was separated
5. washwashed with 100 ml of distilled water
6. dry with materialdried with anhydrous sodium sulfate
7. customby removing the sodium sulfate
8. filtrationby filtration
9. distillationdistilling off the solvent under reduced pressure
10. distillationThe resulting residue was distilled under a reduced pressure of 150 Pa at 30° C.

ORD record

ord-1c58bd53f3f14afa968c57b9eba2f134

Source dataset

uspto-grants-2010_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US07812155B2