Hydrochloric Acid → HCID 59234914, compound

Participants

Reaction Steps

Potassium iodide (1.24 g) and potassium hydroxide (0.46 g) were added to a mixed solution of 4-[1,1,1,3,3,3,-hexafluoro-2-(methoxymethyl)oxypropan-2-yl]phenol (2.50 g, 8.21 mmol) in methanol (63 mL) at room temperature. Then, a 4% sodium hypochlorite solution (15.4 mL) was added in an ice bath over three hours. The mixture was returned to room temperature and stirred overnight. A 1 mol/L sodium thiosulfate aqueous solution was added to the reaction solution at room temperature, and then the pH was adjusted to 7 with 2 mol/L hydrochloric acid. After extraction with diethyl ether-water, the organic layer was concentrated under reduced pressure. The residue was purified by silica gel column chromatography (hexane:ethyl acetate=10:1) to obtain 2.44 g of the title compound (yield: 69%) as a colorless solid.

Provenance & Evidence