Hydrochloric Acid → HCID 56604179, compound

Temperature

15 °C

Add 1.75 g of trimethyl(trifluoromethyl)silane to a solution of 2.1 g of 2,6-dichlorobenzaldehyde in 60 cm3 of dimethoxyethane. The reaction mixture becomes clear with a yellow sheen; it is then cooled on a water/ice bath to about 15° C. Add 0.055 g of caesium fluoride in one go. Stir for 4 hours at a temperature close to 20° C. The reaction mixture is then poured into 7.2 cm3 of a 4N aqueous solution of hydrochloric acid. The aqueous phase is decanted then extracted three times with 40 cm3 of diethyl oxide. The organic phases are combined and then dried over magnesium sulphate, filtered and evaporated to dryness under reduced pressure (2 kPa). We obtain 2.9 g of 1-(2,6-dichlorophenyl)-2,2,2-trifluoroethanol in the form of an oil with a yellow sheen, which has the following characteristics:

1. customclose to 20° C
2. customThe aqueous phase is decanted
3. extractionthen extracted three times with 40 cm3 of diethyl oxide
4. dry with materialdried over magnesium sulphate
5. filtrationfiltered
6. customevaporated to dryness under reduced pressure (2 kPa)

ORD record

ord-fe1c69bd338c41919b1a52c8409a4758

Source dataset

uspto-grants-2012_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08188078B2