Water → HCID 19700289, compound

Participants

Reaction Steps

4.1 g (10 mmol) of 1,3-bis-(2,2,2-trifluoro-1-hydroxy-1-trifluoromethylethyl)-benzene were dissolved in 20 ml of dry DMF, and 0.75 g (25 mmol) of sodium hydride (80% strength dispersion) was added. The clear solution formed was stirred for a further 30 minutes. 4.75 g (25 mmol) of toluene-4-sulfonyl chloride in 15 ml of DMF were added dropwise at 10° to 15° C. The mixture was stirred for 48 hours at room temperature and poured into water. The crystalline precipitate was filtered off, washed with water and dried. The residue was chromatographed over a silica gel column with methylene chloride. 3.5 g of 1,3-bis-[2,2,2-trifluoro-1-(toluene-4-sulfonyloxy)-1-trifluoromethylethyl]-benzene were obtained (colorless crystals, m.p.: 131° C.).

Provenance & Evidence