反应 #1701655
相关文献 (1)
openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08188078B2
反应条件: temp:15.01; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: 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: close to 20° C The aqueous phase is decanted then extracted three times with 40 cm3 of diethyl oxide dried over magnesium sulphate filtered evaporated to dryness under reduced pressure (2 kPa)
来源 ID: ord-fe1c69bd338c41919b1a52c8409a4758