Triethylamine → 1-Methanesulfonyloxy-7,7,8,8,8-pentafluorooctane

Temperature

0 °C

7,7,8,8,8-Pentafluorooctan-1-ol(25 g, 113 mmol) was dissolved in dichloromethane (250 ml), triethylamine(47.4 ml, 339 mmol) and methanesulfonylchloride(17.6 ml, 227 mmol) were added dropwise under cooling to 0° C., and the resulting mixture was stirred for 1 hour. The reaction solution was diluted with water, extracted twice with dichloromethane(200 ml), washed with water and saturated saline solution, dried over anhydrous magnesium sulfate, and filtered. The filtrate was concentrated under reduced pressure and the residue was purified by silica gel column chromatography (eluent:ethyl acetate/n-hexane=1/10, v/v) to give 30 g(100 mmol, Yield 89%) of the title compound.

1. extractionextracted twice with dichloromethane(200 ml)
2. washwashed with water and saturated saline solution
3. dry with materialdried over anhydrous magnesium sulfate
4. filtrationfiltered
5. concentrationThe filtrate was concentrated under reduced pressure
6. customthe residue was purified by silica gel column chromatography (eluent

ORD record

ord-c7ed5dd5fb604b54a3dc17b1c1632a80

Source dataset

uspto-grants-2003_04

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06555571B2