Water → HCID 19700277, 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. 5.25 g (25 mmol) of 4-chlorobenzenesulfonyl chloride in 15 ml of DMF were then 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, rinsed with water and dried. The residue was chromatographed over a silica gel column with methylene chloride. 4.2 g of 1,3-bis-[1-(4-chlorobenzenesulfonyloxy)-2,2,2-trifluoro-1-trifluoromethylethyl]-benzene were obtained (colorless crystals, m.p.: 125° C.).

Provenance & Evidence